# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 _publ_requested_journal CrystEngComm loop_ _publ_author_name 'Wei-Yin Sun.' 'Yong-Qing Huang.' 'Taka-aki Okamura' 'Zhong-Liang Shen.' 'Norikazu Ueyama' 'Jin-Quan Yu.' 'Xia-Ying Zhou.' _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University State Key Laboratory of Coordinatio Nanjing 210093 CHINA ; _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Metal-organic frameworks with oxazoline-containing tripodal ligand: structure changes via reaction medium and metal-to-ligand ratio ; # Attachment 'sunwy.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 765870' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 Cl2 Cu2 N6 O15' _chemical_formula_sum 'C30 H32 Cl2 Cu2 N6 O15' _chemical_formula_weight 914.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9131(8) _cell_length_b 14.4528(9) _cell_length_c 20.5450(10) _cell_angle_alpha 76.2060(10) _cell_angle_beta 74.4060(10) _cell_angle_gamma 64.9360(10) _cell_volume 3567.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7640 _exptl_absorpt_correction_T_max 0.8044 _exptl_absorpt_process_details 'Sadabs (Bruker 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17843 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12317 _reflns_number_gt 8458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker 2000)' _computing_cell_refinement 'SAINT (Bruker 2000)' _computing_data_reduction 'SAINT (Bruker 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+2.9481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12317 _refine_ls_number_parameters 1070 _refine_ls_number_restraints 161 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.82169(5) 0.83010(5) 1.10174(3) 0.04313(19) Uani 1 1 d . . . Cu2 Cu 1.18420(6) 0.61040(5) 1.05761(4) 0.0514(2) Uani 1 1 d . . . Cu3 Cu 0.31111(5) 0.13198(6) 0.35892(3) 0.0483(2) Uani 1 1 d . . . Cu4 Cu 0.28788(6) -0.23722(6) 0.49814(4) 0.0602(2) Uani 1 1 d . . . Cl1 Cl 0.47544(15) 0.24228(19) 0.04000(10) 0.0840(6) Uani 1 1 d . . . Cl2 Cl 0.46331(15) 0.39895(16) 0.29392(13) 0.0914(6) Uani 1 1 d D . . O1 O 1.2341(3) 0.8805(3) 1.0513(2) 0.0540(10) Uani 1 1 d . . . O1W O 1.4005(7) 0.5111(7) 1.0531(5) 0.164(3) Uani 1 1 d . . . O2 O 1.0688(4) 1.0748(4) 0.76910(18) 0.0642(12) Uani 1 1 d . . . O2W O 0.3600(11) -0.4214(10) 0.5759(7) 0.239(5) Uani 1 1 d . . . O3 O 0.8185(3) 0.9179(3) 0.89487(17) 0.0479(9) Uani 1 1 d . . . O4 O 1.1591(3) 0.6682(3) 0.85267(18) 0.0534(10) Uani 1 1 d . . . O5 O 0.8422(4) 0.6358(3) 0.80036(19) 0.0631(12) Uani 1 1 d . . . O6 O 0.7476(3) 0.5725(3) 1.1176(2) 0.0592(11) Uani 1 1 d . . . O7 O 0.1962(3) 0.2196(3) 0.55353(19) 0.0545(10) Uani 1 1 d . . . O8 O 0.6032(3) -0.2580(4) 0.4779(3) 0.0770(13) Uani 1 1 d . . . O9 O 0.3726(3) -0.0342(4) 0.7424(2) 0.0804(15) Uani 1 1 d . . . O10 O -0.1264(4) 0.2935(4) 0.6186(3) 0.0853(16) Uani 1 1 d . . . O11 O 0.1498(3) -0.0590(3) 0.65737(18) 0.0571(10) Uani 1 1 d . . . O12 O 0.0282(3) 0.1261(4) 0.32981(18) 0.0620(11) Uani 1 1 d . . . O13 O 0.3841(5) 0.2836(5) 0.0906(3) 0.112(2) Uani 1 1 d . A . O14 O 0.5656(5) 0.2551(7) 0.0448(4) 0.144(3) Uani 1 1 d . A . O15 O 0.4465(6) 0.2763(8) -0.0246(3) 0.115(5) Uani 0.782(18) 1 d P A 1 O15' O 0.455(3) 0.329(2) 0.028(4) 0.23(4) Uani 0.218(18) 1 d P A 2 O16 O 0.5045(6) 0.1328(5) 0.0526(4) 0.138(3) Uani 1 1 d . A . O17 O 0.3617(17) 0.401(3) 0.3159(13) 0.140(11) Uani 0.51(3) 1 d P B 1 O18 O 0.486(2) 0.4034(18) 0.3575(13) 0.186(17) Uani 0.51(3) 1 d PD B 1 O17' O 0.379(3) 0.390(2) 0.341(2) 0.199(18) Uani 0.49(3) 1 d P B 2 O18' O 0.5357(14) 0.4366(14) 0.2958(13) 0.133(8) Uani 0.49(3) 1 d P B 2 O19 O 0.5321(5) 0.3040(5) 0.2706(3) 0.112(2) Uani 1 1 d . B . O20 O 0.4330(9) 0.4776(8) 0.2432(6) 0.214(5) Uani 1 1 d . B . Cl3 Cl 0.1032(2) 0.5350(2) 0.6610(2) 0.1423(12) Uani 0.599(19) 1 d PDU C 1 O21 O 0.0481(14) 0.6393(7) 0.6711(10) 0.164(10) Uani 0.599(19) 1 d PDU C 1 O22 O 0.2159(6) 0.5050(11) 0.6560(6) 0.133(6) Uani 0.599(19) 1 d PDU C 1 O23 O 0.0684(11) 0.4720(12) 0.7196(10) 0.246(16) Uani 0.599(19) 1 d PDU C 1 O24 O 0.0806(18) 0.5248(19) 0.5997(10) 0.34(2) Uani 0.599(19) 1 d PDU C 1 Cl3' Cl 0.1032(2) 0.5350(2) 0.6610(2) 0.1423(12) Uani 0.401(19) 1 d PDU C 2 O21' O 0.0064(11) 0.6242(10) 0.6652(13) 0.107(8) Uani 0.401(19) 1 d PDU C 2 O22' O 0.164(3) 0.533(3) 0.7074(18) 0.42(4) Uani 0.401(19) 1 d PDU C 2 O23' O 0.094(2) 0.4402(12) 0.6649(10) 0.179(13) Uani 0.401(19) 1 d PDU C 2 O24' O 0.161(3) 0.5537(15) 0.5913(10) 0.34(3) Uani 0.401(19) 1 d PDU C 2 Cl4 Cl 0.3954(5) 0.8425(3) 0.2743(3) 0.212(3) Uani 0.540(17) 1 d PDU D 1 O25 O 0.3860(16) 0.9058(11) 0.2104(5) 0.119(6) Uani 0.540(17) 1 d PDU D 1 O26 O 0.432(2) 0.7363(9) 0.2643(13) 0.35(3) Uani 0.540(17) 1 d PDU D 1 O27 O 0.4791(9) 0.8500(9) 0.3010(6) 0.130(7) Uani 0.540(17) 1 d PDU D 1 O28 O 0.2962(11) 0.8699(12) 0.3221(8) 0.192 Uani 0.54 1 d PDU D 1 Cl4' Cl 0.3954(5) 0.8425(3) 0.2743(3) 0.212(3) Uani 0.460(17) 1 d PDU D 2 O25' O 0.4381(17) 0.8926(18) 0.2126(8) 0.186(15) Uani 0.460(17) 1 d PDU D 2 O26' O 0.4629(14) 0.7356(7) 0.2851(10) 0.137(8) Uani 0.460(17) 1 d PDU D 2 O27' O 0.3864(14) 0.8900(8) 0.3311(6) 0.109 Uani 0.46 1 d PDU D 2 O28' O 0.2840(10) 0.8583(14) 0.2745(9) 0.243(19) Uani 0.460(17) 1 d PDU D 2 N1 N 1.1959(4) 0.7391(4) 1.0769(2) 0.0562(13) Uani 1 1 d . . . N2 N 1.1414(4) 1.1330(3) 0.8265(2) 0.0445(10) Uani 1 1 d . . . N3 N 0.7985(3) 0.8795(3) 1.0084(2) 0.0380(9) Uani 1 1 d . . . N4 N 1.1907(3) 0.6286(3) 0.9594(2) 0.0426(10) Uani 1 1 d . . . N5 N 0.8271(4) 0.4932(3) 0.8646(2) 0.0486(11) Uani 1 1 d . . . N6 N 0.7880(4) 0.7002(4) 1.1305(2) 0.0513(12) Uani 1 1 d . . . N7 N 0.2536(3) 0.1909(3) 0.4448(2) 0.0450(10) Uani 1 1 d . . . N8 N 0.4451(4) -0.2560(4) 0.4715(3) 0.0607(13) Uani 1 1 d . . . N9 N 0.5507(4) -0.1033(4) 0.7041(2) 0.0540(12) Uani 1 1 d . . . N10 N -0.2358(4) 0.2934(4) 0.5566(2) 0.0540(12) Uani 1 1 d . . . N11 N 0.2206(4) -0.1672(4) 0.5800(2) 0.0499(11) Uani 1 1 d . . . N12 N 0.1920(3) 0.1190(3) 0.3280(2) 0.0427(10) Uani 1 1 d . . . C1 C 1.1205(4) 0.8747(4) 0.9850(2) 0.0371(11) Uani 1 1 d . . . C2 C 1.1478(4) 0.9425(4) 0.9307(2) 0.0387(11) Uani 1 1 d . . . H2A H 1.2083 0.9567 0.9275 0.046 Uiso 1 1 calc R . . C3 C 1.0839(4) 0.9892(4) 0.8811(2) 0.0390(11) Uani 1 1 d . . . C4 C 0.9945(4) 0.9668(4) 0.8861(2) 0.0402(12) Uani 1 1 d . . . H4A H 0.9545 0.9950 0.8514 0.048 Uiso 1 1 calc R . . C5 C 0.9637(4) 0.9030(4) 0.9420(2) 0.0360(11) Uani 1 1 d . . . C6 C 1.0273(4) 0.8574(4) 0.9915(2) 0.0382(11) Uani 1 1 d . . . H6A H 1.0073 0.8148 1.0295 0.046 Uiso 1 1 calc R . . C7 C 1.1853(4) 0.8248(4) 1.0398(3) 0.0427(12) Uani 1 1 d . . . C8 C 1.2639(7) 0.7257(6) 1.1250(4) 0.082(2) Uani 1 1 d . . . H8A H 1.3295 0.6642 1.1196 0.099 Uiso 1 1 calc R . . H8B H 1.2251 0.7200 1.1718 0.099 Uiso 1 1 calc R . . C9 C 1.2895(5) 0.8198(5) 1.1076(3) 0.0635(17) Uani 1 1 d . . . H9A H 1.2629 0.8575 1.1463 0.076 Uiso 1 1 calc R . . H9B H 1.3669 0.8020 1.0937 0.076 Uiso 1 1 calc R . . C10 C 1.1027(4) 1.0685(4) 0.8255(2) 0.0419(12) Uani 1 1 d . . . C11 C 1.1433(6) 1.1973(5) 0.7577(3) 0.0661(18) Uani 1 1 d . . . H11A H 1.2169 1.1844 0.7333 0.079 Uiso 1 1 calc R . . H11B H 1.1059 1.2702 0.7615 0.079 Uiso 1 1 calc R . . C12 C 1.0850(7) 1.1624(6) 0.7222(3) 0.076(2) Uani 1 1 d . . . H12A H 1.0163 1.2170 0.7148 0.091 Uiso 1 1 calc R . . H12B H 1.1284 1.1417 0.6786 0.091 Uiso 1 1 calc R . . C13 C 0.8578(4) 0.8970(4) 0.9517(3) 0.0378(11) Uani 1 1 d . . . C14 C 0.6946(4) 0.8939(5) 0.9935(3) 0.0483(13) Uani 1 1 d . . . H14A H 0.6364 0.9538 1.0116 0.058 Uiso 1 1 calc R . . H14B H 0.6770 0.8336 1.0127 0.058 Uiso 1 1 calc R . . C15 C 0.7135(5) 0.9094(5) 0.9165(3) 0.0598(16) Uani 1 1 d . . . H15A H 0.7147 0.8511 0.9002 0.072 Uiso 1 1 calc R . . H15B H 0.6575 0.9717 0.8996 0.072 Uiso 1 1 calc R . . C16 C 1.0205(4) 0.6352(4) 0.9397(2) 0.0369(11) Uani 1 1 d . . . C17 C 0.9809(4) 0.6170(4) 0.8907(3) 0.0387(11) Uani 1 1 d . . . H17A H 1.0171 0.6178 0.8455 0.046 Uiso 1 1 calc R . . C18 C 0.8875(4) 0.5977(4) 0.9098(2) 0.0392(11) Uani 1 1 d . . . C19 C 0.8299(4) 0.6006(4) 0.9760(3) 0.0391(11) Uani 1 1 d . . . H19A H 0.7670 0.5875 0.9882 0.047 Uiso 1 1 calc R . . C20 C 0.8672(4) 0.6237(4) 1.0246(2) 0.0371(11) Uani 1 1 d . . . C21 C 0.9637(4) 0.6386(4) 1.0063(2) 0.0391(11) Uani 1 1 d . . . H21A H 0.9903 0.6510 1.0389 0.047 Uiso 1 1 calc R . . C22 C 1.1272(4) 0.6439(4) 0.9199(3) 0.0404(12) Uani 1 1 d . . . C23 C 1.2917(5) 0.6344(5) 0.9151(3) 0.0566(15) Uani 1 1 d . . . H23A H 1.3505 0.5671 0.9167 0.068 Uiso 1 1 calc R . . H23B H 1.3119 0.6824 0.9287 0.068 Uiso 1 1 calc R . . C24 C 1.2645(5) 0.6719(6) 0.8445(3) 0.0720(19) Uani 1 1 d . . . H24A H 1.2615 0.7417 0.8287 0.086 Uiso 1 1 calc R . . H24B H 1.3178 0.6273 0.8122 0.086 Uiso 1 1 calc R . . C25 C 0.8502(4) 0.5713(4) 0.8583(3) 0.0424(12) Uani 1 1 d . . . C26 C 0.7960(7) 0.4978(6) 0.8000(3) 0.076(2) Uani 1 1 d . . . H26A H 0.7241 0.4976 0.8085 0.092 Uiso 1 1 calc R . . H26B H 0.8467 0.4399 0.7765 0.092 Uiso 1 1 calc R . . C27 C 0.7992(7) 0.5990(6) 0.7585(3) 0.081(2) Uani 1 1 d . . . H27A H 0.8462 0.5881 0.7142 0.097 Uiso 1 1 calc R . . H27B H 0.7274 0.6476 0.7519 0.097 Uiso 1 1 calc R . . C28 C 0.8010(4) 0.6352(4) 1.0939(3) 0.0422(12) Uani 1 1 d . . . C29 C 0.7126(6) 0.6846(6) 1.1942(3) 0.074(2) Uani 1 1 d . . . H29A H 0.6499 0.7479 1.2016 0.089 Uiso 1 1 calc R . . H29B H 0.7479 0.6613 1.2333 0.089 Uiso 1 1 calc R . . C30 C 0.6811(7) 0.6035(7) 1.1830(4) 0.091(3) Uani 1 1 d . . . H30A H 0.6958 0.5453 1.2193 0.110 Uiso 1 1 calc R . . H30B H 0.6049 0.6312 1.1812 0.110 Uiso 1 1 calc R . . C31 C 0.3315(4) 0.0536(4) 0.5349(3) 0.0418(12) Uani 1 1 d . . . C32 C 0.3778(4) -0.0290(4) 0.4985(3) 0.0456(13) Uani 1 1 d . . . H32A H 0.3616 -0.0212 0.4559 0.055 Uiso 1 1 calc R . . C33 C 0.4488(4) -0.1242(4) 0.5254(3) 0.0461(13) Uani 1 1 d . . . C34 C 0.4757(4) -0.1336(5) 0.5877(3) 0.0503(14) Uani 1 1 d . . . H34A H 0.5255 -0.1957 0.6050 0.060 Uiso 1 1 calc R . . C35 C 0.4292(4) -0.0512(5) 0.6241(3) 0.0480(14) Uani 1 1 d . . . C36 C 0.3560(4) 0.0417(4) 0.5987(3) 0.0463(13) Uani 1 1 d . . . H36A H 0.3231 0.0963 0.6240 0.056 Uiso 1 1 calc R . . C37 C 0.2600(4) 0.1557(4) 0.5074(3) 0.0432(12) Uani 1 1 d . . . C38 C 0.1777(5) 0.2996(5) 0.4414(3) 0.0573(15) Uani 1 1 d . . . H38A H 0.1193 0.3114 0.4192 0.069 Uiso 1 1 calc R . . H38B H 0.2144 0.3453 0.4168 0.069 Uiso 1 1 calc R . . C39 C 0.1354(5) 0.3159(5) 0.5159(3) 0.0620(16) Uani 1 1 d . . . H39A H 0.1478 0.3728 0.5244 0.074 Uiso 1 1 calc R . . H39B H 0.0586 0.3303 0.5285 0.074 Uiso 1 1 calc R . . C40 C 0.4949(4) -0.2137(5) 0.4899(3) 0.0505(14) Uani 1 1 d . . . C41 C 0.5270(5) -0.3453(6) 0.4393(4) 0.082(2) Uani 1 1 d . . . H41A H 0.5226 -0.3374 0.3919 0.098 Uiso 1 1 calc R . . H41B H 0.5185 -0.4087 0.4631 0.098 Uiso 1 1 calc R . . C42 C 0.6323(6) -0.3452(7) 0.4453(5) 0.095(3) Uani 1 1 d . . . H42A H 0.6717 -0.4083 0.4725 0.114 Uiso 1 1 calc R . . H42B H 0.6771 -0.3390 0.4006 0.114 Uiso 1 1 calc R . . C43 C 0.4566(5) -0.0643(5) 0.6910(3) 0.0541(15) Uani 1 1 d . . . C44 C 0.5377(5) -0.1071(7) 0.7788(3) 0.077(2) Uani 1 1 d . . . H44A H 0.5663 -0.1778 0.8010 0.092 Uiso 1 1 calc R . . H44B H 0.5743 -0.0689 0.7880 0.092 Uiso 1 1 calc R . . C45 C 0.4192(5) -0.0584(7) 0.8025(3) 0.078 Uani 1 1 d . . . H45A H 0.3933 -0.1056 0.8372 0.093 Uiso 1 1 calc R . . H45B H 0.4006 0.0038 0.8214 0.093 Uiso 1 1 calc R . . C46 C -0.0466(4) 0.1748(4) 0.5385(3) 0.0427(12) Uani 1 1 d . . . C47 C 0.0149(4) 0.0917(4) 0.5784(3) 0.0446(13) Uani 1 1 d . . . H47A H -0.0024 0.0887 0.6256 0.053 Uiso 1 1 calc R . . C48 C 0.1029(4) 0.0119(4) 0.5487(3) 0.0400(12) Uani 1 1 d . . . C49 C 0.1305(4) 0.0190(4) 0.4778(2) 0.0390(11) Uani 1 1 d . . . H49A H 0.1889 -0.0338 0.4573 0.047 Uiso 1 1 calc R . . C50 C 0.0703(4) 0.1055(4) 0.4382(2) 0.0385(11) Uani 1 1 d . . . C51 C -0.0195(4) 0.1818(4) 0.4678(3) 0.0429(12) Uani 1 1 d . . . H51A H -0.0616 0.2376 0.4407 0.051 Uiso 1 1 calc R . . C52 C -0.1422(5) 0.2561(5) 0.5707(3) 0.0524(14) Uani 1 1 d . . . C53 C -0.3029(6) 0.3761(6) 0.5979(4) 0.081(2) Uani 1 1 d . . . H53A H -0.3674 0.3654 0.6244 0.098 Uiso 1 1 calc R . . H53B H -0.3241 0.4426 0.5692 0.098 Uiso 1 1 calc R . . C54 C -0.2311(5) 0.3704(6) 0.6446(4) 0.080 Uani 1 1 d . . . H54A H -0.2265 0.4366 0.6411 0.096 Uiso 1 1 calc R . . H54B H -0.2580 0.3483 0.6918 0.096 Uiso 1 1 calc R . . C55 C 0.1629(4) -0.0779(4) 0.5934(3) 0.0432(12) Uani 1 1 d . . . C56 C 0.2094(5) -0.1551(6) 0.6951(3) 0.069(2) Uani 1 1 d . . . H56A H 0.1621 -0.1760 0.7344 0.083 Uiso 1 1 calc R . . H56B H 0.2664 -0.1496 0.7106 0.083 Uiso 1 1 calc R . . C57 C 0.2551(6) -0.2297(6) 0.6451(4) 0.075(2) Uani 1 1 d . . . H57A H 0.2268 -0.2838 0.6604 0.090 Uiso 1 1 calc R . . H57B H 0.3333 -0.2611 0.6390 0.090 Uiso 1 1 calc R . . C58 C 0.1031(4) 0.1168(4) 0.3624(3) 0.0414(12) Uani 1 1 d . . . C59 C 0.1877(5) 0.1258(5) 0.2558(3) 0.0505(14) Uani 1 1 d . . . H59A H 0.2367 0.0620 0.2380 0.061 Uiso 1 1 calc R . . H59B H 0.2063 0.1823 0.2277 0.061 Uiso 1 1 calc R . . C60 C 0.0722(5) 0.1444(7) 0.2576(3) 0.084(2) Uani 1 1 d . . . H60A H 0.0336 0.2147 0.2380 0.101 Uiso 1 1 calc R . . H60B H 0.0684 0.0971 0.2328 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0538(4) 0.0483(4) 0.0361(3) -0.0067(3) -0.0062(3) -0.0290(3) Cu2 0.0671(5) 0.0485(4) 0.0517(4) 0.0060(3) -0.0261(3) -0.0326(4) Cu3 0.0439(4) 0.0615(5) 0.0407(4) 0.0002(3) -0.0092(3) -0.0247(3) Cu4 0.0496(4) 0.0564(5) 0.0804(5) -0.0092(4) -0.0222(4) -0.0203(4) Cl1 0.0692(12) 0.1057(17) 0.0789(12) 0.0015(11) -0.0223(10) -0.0381(11) Cl2 0.0584(11) 0.0657(12) 0.138(2) -0.0035(12) -0.0228(12) -0.0155(9) O1 0.061(2) 0.044(2) 0.073(3) -0.0061(19) -0.027(2) -0.0274(19) O1W 0.139(6) 0.165(8) 0.186(8) -0.042(6) 0.006(6) -0.070(6) O2 0.101(3) 0.093(3) 0.033(2) 0.001(2) -0.016(2) -0.074(3) O2W 0.264(13) 0.213(12) 0.250(13) -0.066(10) -0.049(10) -0.082(10) O3 0.056(2) 0.067(2) 0.0352(19) -0.0040(17) -0.0118(16) -0.037(2) O4 0.059(2) 0.069(3) 0.043(2) 0.0011(19) -0.0117(18) -0.038(2) O5 0.102(3) 0.066(3) 0.046(2) 0.014(2) -0.033(2) -0.056(3) O6 0.077(3) 0.064(3) 0.053(2) -0.011(2) 0.003(2) -0.050(2) O7 0.051(2) 0.065(3) 0.045(2) -0.007(2) -0.0079(18) -0.022(2) O8 0.042(2) 0.085(3) 0.111(4) -0.038(3) -0.008(2) -0.024(2) O9 0.042(2) 0.141(5) 0.044(2) -0.011(3) -0.0046(18) -0.024(3) O10 0.062(3) 0.105(4) 0.102(4) -0.064(3) -0.026(3) -0.014(3) O11 0.067(3) 0.077(3) 0.037(2) 0.0064(19) -0.0230(18) -0.037(2) O12 0.057(2) 0.108(3) 0.038(2) 0.001(2) -0.0167(18) -0.048(2) O13 0.081(4) 0.122(5) 0.091(4) -0.009(4) -0.014(3) -0.006(4) O14 0.098(5) 0.191(7) 0.197(7) -0.076(6) -0.016(5) -0.088(5) O15 0.103(6) 0.168(10) 0.057(4) 0.020(5) -0.029(4) -0.047(5) O15' 0.09(2) 0.07(2) 0.59(11) -0.13(4) -0.08(4) -0.022(18) O16 0.154(6) 0.089(5) 0.178(7) -0.020(5) -0.040(5) -0.047(5) O17 0.055(9) 0.23(3) 0.150(18) -0.093(17) -0.025(11) -0.030(11) O18 0.16(2) 0.172(18) 0.21(3) -0.132(19) -0.15(2) 0.065(15) O17' 0.16(3) 0.102(14) 0.23(3) -0.024(17) 0.12(2) -0.047(16) O18' 0.138(13) 0.159(15) 0.141(18) -0.054(12) -0.028(11) -0.076(12) O19 0.099(4) 0.091(4) 0.131(5) -0.028(4) 0.015(4) -0.039(4) O20 0.189(9) 0.168(9) 0.256(12) 0.061(9) -0.089(9) -0.062(7) Cl3 0.098(2) 0.089(2) 0.215(4) -0.023(2) -0.026(2) -0.0153(16) O21 0.123(13) 0.121(12) 0.191(18) -0.032(11) 0.060(13) -0.043(10) O22 0.106(9) 0.154(13) 0.100(10) -0.015(9) -0.015(7) -0.018(8) O23 0.134(13) 0.095(11) 0.45(4) 0.107(18) -0.080(18) -0.047(10) O24 0.29(3) 0.25(3) 0.54(5) -0.16(3) -0.28(3) 0.01(2) Cl3' 0.098(2) 0.089(2) 0.215(4) -0.023(2) -0.026(2) -0.0153(16) O21' 0.083(12) 0.066(10) 0.152(17) 0.012(10) -0.019(12) -0.025(9) O22' 0.33(5) 0.51(8) 0.41(7) 0.23(6) -0.19(5) -0.21(5) O23' 0.35(4) 0.120(18) 0.082(13) 0.010(11) -0.016(16) -0.14(2) O24' 0.44(5) 0.072(14) 0.27(4) -0.014(19) 0.22(4) -0.04(2) Cl4 0.253(6) 0.093(3) 0.184(5) 0.021(3) 0.001(5) -0.014(4) O25 0.167(17) 0.081(9) 0.100(10) 0.027(7) -0.049(9) -0.048(10) O26 0.29(3) 0.094(18) 0.35(4) 0.09(2) 0.11(3) 0.044(18) O27 0.151(13) 0.079(9) 0.076(8) -0.010(6) -0.012(8) 0.029(8) O28 0.147 0.152 0.154 -0.053 0.096 0.001 Cl4' 0.253(6) 0.093(3) 0.184(5) 0.021(3) 0.001(5) -0.014(4) O25' 0.127(18) 0.17(2) 0.17(2) 0.091(16) -0.012(13) -0.042(14) O26' 0.148(15) 0.046(10) 0.145(15) -0.009(9) 0.053(12) -0.019(10) O27' 0.199 0.061 0.101 -0.006 -0.107 -0.037 O28' 0.46(5) 0.100(14) 0.066(11) -0.027(10) 0.002(18) -0.04(2) N1 0.081(3) 0.048(3) 0.059(3) 0.003(2) -0.032(3) -0.038(3) N2 0.062(3) 0.048(3) 0.031(2) -0.0016(19) -0.0039(19) -0.033(2) N3 0.042(2) 0.041(2) 0.037(2) -0.0019(18) -0.0084(18) -0.024(2) N4 0.045(2) 0.038(2) 0.052(3) -0.004(2) -0.014(2) -0.021(2) N5 0.068(3) 0.049(3) 0.046(3) 0.004(2) -0.028(2) -0.035(2) N6 0.080(3) 0.051(3) 0.038(2) -0.005(2) -0.004(2) -0.044(3) N7 0.045(2) 0.055(3) 0.042(3) 0.000(2) -0.0105(19) -0.028(2) N8 0.045(3) 0.072(3) 0.070(3) -0.018(3) -0.010(2) -0.024(3) N9 0.042(3) 0.079(3) 0.041(3) 0.000(2) -0.010(2) -0.026(2) N10 0.046(3) 0.058(3) 0.058(3) -0.014(2) -0.009(2) -0.018(2) N11 0.047(3) 0.057(3) 0.052(3) 0.008(2) -0.023(2) -0.026(2) N12 0.045(2) 0.054(3) 0.031(2) -0.0031(19) -0.0062(18) -0.023(2) C1 0.042(3) 0.032(3) 0.042(3) -0.015(2) -0.004(2) -0.015(2) C2 0.046(3) 0.038(3) 0.040(3) -0.013(2) -0.003(2) -0.023(2) C3 0.049(3) 0.036(3) 0.038(3) -0.012(2) 0.001(2) -0.024(2) C4 0.045(3) 0.047(3) 0.037(3) -0.011(2) -0.005(2) -0.025(2) C5 0.045(3) 0.037(3) 0.032(3) -0.008(2) -0.004(2) -0.022(2) C6 0.048(3) 0.032(3) 0.038(3) -0.006(2) -0.004(2) -0.020(2) C7 0.049(3) 0.039(3) 0.048(3) -0.008(2) -0.012(2) -0.021(2) C8 0.129(6) 0.072(5) 0.079(5) 0.019(4) -0.067(5) -0.058(5) C9 0.072(4) 0.059(4) 0.075(4) 0.004(3) -0.036(3) -0.033(3) C10 0.048(3) 0.054(3) 0.032(3) -0.013(2) -0.001(2) -0.029(3) C11 0.099(5) 0.079(4) 0.046(3) 0.011(3) -0.024(3) -0.062(4) C12 0.112(6) 0.106(6) 0.041(3) 0.015(3) -0.023(3) -0.079(5) C13 0.045(3) 0.032(3) 0.042(3) -0.005(2) -0.012(2) -0.019(2) C14 0.044(3) 0.059(4) 0.046(3) -0.001(3) -0.013(2) -0.025(3) C15 0.062(4) 0.085(5) 0.050(3) 0.001(3) -0.016(3) -0.047(4) C16 0.038(3) 0.031(3) 0.042(3) -0.003(2) -0.009(2) -0.013(2) C17 0.048(3) 0.034(3) 0.037(3) 0.000(2) -0.011(2) -0.019(2) C18 0.051(3) 0.035(3) 0.038(3) 0.001(2) -0.017(2) -0.020(2) C19 0.041(3) 0.034(3) 0.047(3) -0.001(2) -0.012(2) -0.020(2) C20 0.043(3) 0.031(3) 0.038(3) -0.002(2) -0.009(2) -0.015(2) C21 0.049(3) 0.032(3) 0.041(3) -0.002(2) -0.015(2) -0.018(2) C22 0.046(3) 0.034(3) 0.045(3) -0.004(2) -0.011(2) -0.018(2) C23 0.051(3) 0.068(4) 0.061(4) -0.008(3) -0.008(3) -0.034(3) C24 0.063(4) 0.101(5) 0.067(4) -0.001(4) -0.006(3) -0.054(4) C25 0.049(3) 0.043(3) 0.038(3) 0.000(2) -0.014(2) -0.021(3) C26 0.126(6) 0.085(5) 0.055(4) 0.014(3) -0.051(4) -0.068(5) C27 0.127(6) 0.095(5) 0.057(4) 0.015(4) -0.049(4) -0.072(5) C28 0.050(3) 0.044(3) 0.039(3) 0.002(2) -0.009(2) -0.027(3) C29 0.104(5) 0.085(5) 0.049(4) -0.014(3) 0.014(3) -0.065(5) C30 0.133(7) 0.106(6) 0.060(4) -0.033(4) 0.031(4) -0.088(6) C31 0.035(3) 0.053(3) 0.043(3) -0.002(3) -0.007(2) -0.025(2) C32 0.038(3) 0.066(4) 0.043(3) 0.000(3) -0.008(2) -0.034(3) C33 0.039(3) 0.057(3) 0.049(3) -0.005(3) -0.005(2) -0.028(3) C34 0.040(3) 0.065(4) 0.050(3) 0.006(3) -0.013(2) -0.029(3) C35 0.039(3) 0.069(4) 0.041(3) 0.006(3) -0.009(2) -0.032(3) C36 0.042(3) 0.058(3) 0.042(3) -0.004(3) -0.004(2) -0.027(3) C37 0.038(3) 0.055(3) 0.044(3) -0.008(3) -0.006(2) -0.026(3) C38 0.059(4) 0.055(4) 0.058(4) 0.003(3) -0.020(3) -0.022(3) C39 0.056(4) 0.066(4) 0.067(4) -0.008(3) -0.017(3) -0.025(3) C40 0.042(3) 0.057(4) 0.054(3) -0.001(3) -0.007(3) -0.025(3) C41 0.055(4) 0.083(5) 0.111(6) -0.039(5) -0.006(4) -0.023(4) C42 0.050(4) 0.093(6) 0.146(8) -0.059(6) -0.007(4) -0.017(4) C43 0.050(3) 0.077(4) 0.041(3) 0.004(3) -0.010(3) -0.035(3) C44 0.053(4) 0.127(6) 0.039(3) -0.009(4) -0.010(3) -0.025(4) C45 0.045 0.145 0.033 -0.021 -0.009 -0.022 C46 0.040(3) 0.053(3) 0.046(3) -0.008(3) -0.013(2) -0.025(3) C47 0.043(3) 0.063(4) 0.040(3) -0.008(3) -0.009(2) -0.032(3) C48 0.040(3) 0.048(3) 0.040(3) 0.001(2) -0.013(2) -0.025(2) C49 0.039(3) 0.051(3) 0.037(3) -0.006(2) -0.010(2) -0.024(2) C50 0.042(3) 0.047(3) 0.034(3) 0.002(2) -0.011(2) -0.026(3) C51 0.041(3) 0.048(3) 0.048(3) 0.000(2) -0.019(2) -0.023(3) C52 0.051(3) 0.062(4) 0.049(3) -0.014(3) -0.009(3) -0.023(3) C53 0.062(4) 0.083(5) 0.093(5) -0.036(4) -0.012(4) -0.012(4) C54 0.063 0.076 0.092 -0.028 -0.007 -0.014 C55 0.040(3) 0.054(4) 0.040(3) 0.004(3) -0.009(2) -0.028(3) C56 0.068(4) 0.101(5) 0.047(4) 0.023(4) -0.029(3) -0.048(4) C57 0.069(4) 0.076(5) 0.083(5) 0.034(4) -0.040(4) -0.038(4) C58 0.044(3) 0.045(3) 0.038(3) 0.001(2) -0.016(2) -0.018(2) C59 0.059(3) 0.060(4) 0.036(3) 0.002(3) -0.013(2) -0.027(3) C60 0.071(4) 0.145(7) 0.044(4) 0.003(4) -0.015(3) -0.055(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.933(4) 2_777 ? Cu1 N3 1.942(4) . ? Cu1 N6 2.040(4) . ? Cu2 N5 1.935(4) 2_767 ? Cu2 N4 1.953(4) . ? Cu2 N1 2.070(4) . ? Cu3 N9 1.946(4) 2_656 ? Cu3 N7 1.965(4) . ? Cu3 N12 2.018(4) . ? Cu4 N10 1.956(5) 2_556 ? Cu4 N11 1.973(5) . ? Cu4 N8 2.021(5) . ? Cl1 O15' 1.14(3) . ? Cl1 O14 1.375(6) . ? Cl1 O15 1.405(6) . ? Cl1 O13 1.412(6) . ? Cl1 O16 1.433(7) . ? Cl2 O17' 1.34(2) . ? Cl2 O18' 1.344(15) . ? Cl2 O20 1.349(10) . ? Cl2 O17 1.35(2) . ? Cl2 O19 1.408(6) . ? Cl2 O18 1.448(9) . ? O1 C7 1.342(6) . ? O1 C9 1.458(7) . ? O2 C10 1.334(6) . ? O2 C12 1.457(7) . ? O3 C13 1.337(6) . ? O3 C15 1.458(6) . ? O4 C22 1.342(6) . ? O4 C24 1.454(7) . ? O5 C25 1.325(6) . ? O5 C27 1.465(7) . ? O6 C28 1.333(6) . ? O6 C30 1.459(7) . ? O7 C37 1.345(6) . ? O7 C39 1.447(7) . ? O8 C40 1.342(7) . ? O8 C42 1.423(8) . ? O9 C43 1.340(7) . ? O9 C45 1.450(7) . ? O10 C52 1.334(7) . ? O10 C54 1.461(8) . ? O11 C55 1.354(6) . ? O11 C56 1.441(7) . ? O12 C58 1.330(6) . ? O12 C60 1.452(7) . ? O13 O15' 1.58(6) . ? O14 O15' 1.53(4) . ? Cl3 O21 1.410(8) . ? Cl3 O22 1.420(8) . ? Cl3 O24 1.430(9) . ? Cl3 O23 1.432(8) . ? Cl4 O25 1.413(8) . ? Cl4 O28 1.421(7) . ? Cl4 O26 1.445(9) . ? Cl4 O27 1.465(8) . ? N1 C7 1.262(7) . ? N1 C8 1.472(7) . ? N2 C10 1.265(6) . ? N2 C11 1.495(7) . ? N2 Cu1 1.933(4) 2_777 ? N3 C13 1.273(6) . ? N3 C14 1.478(6) . ? N4 C22 1.274(6) . ? N4 C23 1.478(7) . ? N5 C25 1.270(7) . ? N5 C26 1.482(7) . ? N5 Cu2 1.935(4) 2_767 ? N6 C28 1.266(7) . ? N6 C29 1.478(7) . ? N7 C37 1.277(6) . ? N7 C38 1.473(7) . ? N8 C40 1.266(7) . ? N8 C41 1.469(8) . ? N9 C43 1.262(7) . ? N9 C44 1.487(7) . ? N9 Cu3 1.946(4) 2_656 ? N10 C52 1.266(7) . ? N10 C53 1.460(8) . ? N10 Cu4 1.956(5) 2_556 ? N11 C55 1.249(7) . ? N11 C57 1.495(7) . ? N12 C58 1.259(6) . ? N12 C59 1.479(6) . ? C1 C2 1.383(7) . ? C1 C6 1.389(7) . ? C1 C7 1.487(7) . ? C2 C3 1.392(7) . ? C2 H2A 0.9300 . ? C3 C4 1.385(7) . ? C3 C10 1.468(7) . ? C4 C5 1.386(7) . ? C4 H4A 0.9300 . ? C5 C6 1.386(7) . ? C5 C13 1.470(7) . ? C6 H6A 0.9300 . ? C8 C9 1.489(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.511(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.509(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.383(7) . ? C16 C17 1.391(7) . ? C16 C22 1.481(7) . ? C17 C18 1.380(7) . ? C17 H17A 0.9300 . ? C18 C19 1.381(7) . ? C18 C25 1.478(7) . ? C19 C20 1.401(7) . ? C19 H19A 0.9300 . ? C20 C21 1.387(7) . ? C20 C28 1.477(7) . ? C21 H21A 0.9300 . ? C23 C24 1.512(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C26 C27 1.519(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 C30 1.496(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.385(8) . ? C31 C36 1.394(7) . ? C31 C37 1.465(7) . ? C32 C33 1.398(8) . ? C32 H32A 0.9300 . ? C33 C34 1.389(7) . ? C33 C40 1.453(8) . ? C34 C35 1.381(8) . ? C34 H34A 0.9300 . ? C35 C36 1.380(8) . ? C35 C43 1.473(8) . ? C36 H36A 0.9300 . ? C38 C39 1.522(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C42 1.503(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C44 C45 1.483(8) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.371(7) . ? C46 C51 1.391(7) . ? C46 C52 1.470(8) . ? C47 C48 1.393(7) . ? C47 H47A 0.9300 . ? C48 C49 1.392(7) . ? C48 C55 1.467(7) . ? C49 C50 1.386(7) . ? C49 H49A 0.9300 . ? C50 C51 1.374(7) . ? C50 C58 1.491(7) . ? C51 H51A 0.9300 . ? C53 C54 1.527(10) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C56 C57 1.490(10) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C59 C60 1.503(8) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 140.91(17) 2_777 . ? N2 Cu1 N6 113.51(17) 2_777 . ? N3 Cu1 N6 105.50(17) . . ? N5 Cu2 N4 137.00(18) 2_767 . ? N5 Cu2 N1 116.42(18) 2_767 . ? N4 Cu2 N1 106.57(18) . . ? N9 Cu3 N7 132.60(19) 2_656 . ? N9 Cu3 N12 116.93(18) 2_656 . ? N7 Cu3 N12 109.88(17) . . ? N10 Cu4 N11 133.74(19) 2_556 . ? N10 Cu4 N8 117.0(2) 2_556 . ? N11 Cu4 N8 109.2(2) . . ? O15' Cl1 O14 74.4(17) . . ? O15' Cl1 O15 72(3) . . ? O14 Cl1 O15 115.2(5) . . ? O15' Cl1 O13 76(3) . . ? O14 Cl1 O13 113.9(5) . . ? O15 Cl1 O13 109.7(4) . . ? O15' Cl1 O16 178(3) . . ? O14 Cl1 O16 104.6(5) . . ? O15 Cl1 O16 106.5(6) . . ? O13 Cl1 O16 106.2(5) . . ? O17' Cl2 O18' 130.2(18) . . ? O17' Cl2 O20 112.7(17) . . ? O18' Cl2 O20 85.8(11) . . ? O17' Cl2 O17 26(2) . . ? O18' Cl2 O17 147.5(15) . . ? O20 Cl2 O17 92.0(13) . . ? O17' Cl2 O19 111.2(12) . . ? O18' Cl2 O19 101.0(8) . . ? O20 Cl2 O19 113.7(7) . . ? O17 Cl2 O19 109.5(14) . . ? O17' Cl2 O18 75.5(18) . . ? O18' Cl2 O18 57.8(12) . . ? O20 Cl2 O18 127.1(13) . . ? O17 Cl2 O18 99.9(16) . . ? O19 Cl2 O18 110.3(6) . . ? C7 O1 C9 105.9(4) . . ? C10 O2 C12 106.8(4) . . ? C13 O3 C15 106.1(4) . . ? C22 O4 C24 105.8(4) . . ? C25 O5 C27 106.8(4) . . ? C28 O6 C30 105.6(4) . . ? C37 O7 C39 106.8(4) . . ? C40 O8 C42 106.6(5) . . ? C43 O9 C45 105.6(4) . . ? C52 O10 C54 106.4(5) . . ? C55 O11 C56 106.7(5) . . ? C58 O12 C60 105.7(4) . . ? Cl1 O13 O15' 44.2(11) . . ? Cl1 O14 O15' 45.8(10) . . ? Cl1 O15' O14 59.8(18) . . ? Cl1 O15' O13 60(3) . . ? O14 O15' O13 97(4) . . ? O21 Cl3 O22 110.0(9) . . ? O21 Cl3 O24 107.8(11) . . ? O22 Cl3 O24 111.0(10) . . ? O21 Cl3 O23 108.9(10) . . ? O22 Cl3 O23 106.7(8) . . ? O24 Cl3 O23 112.5(11) . . ? O25 Cl4 O28 112.3(10) . . ? O25 Cl4 O26 108.7(11) . . ? O28 Cl4 O26 110.0(11) . . ? O25 Cl4 O27 109.0(9) . . ? O28 Cl4 O27 110.0(10) . . ? O26 Cl4 O27 106.8(11) . . ? C7 N1 C8 106.5(5) . . ? C7 N1 Cu2 130.0(4) . . ? C8 N1 Cu2 119.1(4) . . ? C10 N2 C11 107.2(4) . . ? C10 N2 Cu1 133.2(4) . 2_777 ? C11 N2 Cu1 119.1(3) . 2_777 ? C13 N3 C14 107.2(4) . . ? C13 N3 Cu1 134.3(3) . . ? C14 N3 Cu1 118.4(3) . . ? C22 N4 C23 106.6(4) . . ? C22 N4 Cu2 137.2(4) . . ? C23 N4 Cu2 116.0(3) . . ? C25 N5 C26 107.0(4) . . ? C25 N5 Cu2 130.8(4) . 2_767 ? C26 N5 Cu2 121.9(4) . 2_767 ? C28 N6 C29 106.8(4) . . ? C28 N6 Cu1 128.4(4) . . ? C29 N6 Cu1 122.5(4) . . ? C37 N7 C38 107.7(5) . . ? C37 N7 Cu3 135.3(4) . . ? C38 N7 Cu3 116.8(3) . . ? C40 N8 C41 107.3(5) . . ? C40 N8 Cu4 130.0(4) . . ? C41 N8 Cu4 121.1(4) . . ? C43 N9 C44 106.6(5) . . ? C43 N9 Cu3 128.9(4) . 2_656 ? C44 N9 Cu3 123.6(4) . 2_656 ? C52 N10 C53 107.2(5) . . ? C52 N10 Cu4 126.6(4) . 2_556 ? C53 N10 Cu4 125.6(4) . 2_556 ? C55 N11 C57 106.0(5) . . ? C55 N11 Cu4 137.5(4) . . ? C57 N11 Cu4 115.9(4) . . ? C58 N12 C59 106.2(4) . . ? C58 N12 Cu3 128.9(4) . . ? C59 N12 Cu3 124.4(3) . . ? C2 C1 C6 120.2(5) . . ? C2 C1 C7 121.1(4) . . ? C6 C1 C7 118.6(4) . . ? C1 C2 C3 119.4(5) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 C10 117.8(5) . . ? C2 C3 C10 122.2(4) . . ? C3 C4 C5 121.0(5) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 118.7(4) . . ? C4 C5 C13 119.0(4) . . ? C6 C5 C13 121.8(4) . . ? C5 C6 C1 120.7(5) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? N1 C7 O1 118.1(5) . . ? N1 C7 C1 127.1(5) . . ? O1 C7 C1 114.8(4) . . ? N1 C8 C9 105.3(5) . . ? N1 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? N1 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? O1 C9 C8 104.2(5) . . ? O1 C9 H9A 110.9 . . ? C8 C9 H9A 110.9 . . ? O1 C9 H9B 110.9 . . ? C8 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? N2 C10 O2 117.8(5) . . ? N2 C10 C3 127.8(5) . . ? O2 C10 C3 114.3(4) . . ? N2 C11 C12 103.5(4) . . ? N2 C11 H11A 111.1 . . ? C12 C11 H11A 111.1 . . ? N2 C11 H11B 111.1 . . ? C12 C11 H11B 111.1 . . ? H11A C11 H11B 109.0 . . ? O2 C12 C11 104.2(4) . . ? O2 C12 H12A 110.9 . . ? C11 C12 H12A 110.9 . . ? O2 C12 H12B 110.9 . . ? C11 C12 H12B 110.9 . . ? H12A C12 H12B 108.9 . . ? N3 C13 O3 117.7(4) . . ? N3 C13 C5 126.6(4) . . ? O3 C13 C5 115.6(4) . . ? N3 C14 C15 103.9(4) . . ? N3 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? N3 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? O3 C15 C14 104.3(4) . . ? O3 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? O3 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? C21 C16 C17 120.1(4) . . ? C21 C16 C22 121.4(4) . . ? C17 C16 C22 118.4(4) . . ? C18 C17 C16 119.3(5) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 121.2(5) . . ? C17 C18 C25 118.9(5) . . ? C19 C18 C25 119.8(4) . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C21 C20 C19 119.6(5) . . ? C21 C20 C28 121.2(4) . . ? C19 C20 C28 119.2(4) . . ? C16 C21 C20 120.4(5) . . ? C16 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? N4 C22 O4 118.2(5) . . ? N4 C22 C16 127.0(5) . . ? O4 C22 C16 114.8(4) . . ? N4 C23 C24 104.1(4) . . ? N4 C23 H23A 110.9 . . ? C24 C23 H23A 110.9 . . ? N4 C23 H23B 110.9 . . ? C24 C23 H23B 110.9 . . ? H23A C23 H23B 109.0 . . ? O4 C24 C23 104.5(5) . . ? O4 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? O4 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? N5 C25 O5 118.2(5) . . ? N5 C25 C18 126.2(4) . . ? O5 C25 C18 115.6(4) . . ? N5 C26 C27 104.2(5) . . ? N5 C26 H26A 110.9 . . ? C27 C26 H26A 110.9 . . ? N5 C26 H26B 110.9 . . ? C27 C26 H26B 110.9 . . ? H26A C26 H26B 108.9 . . ? O5 C27 C26 103.4(4) . . ? O5 C27 H27A 111.1 . . ? C26 C27 H27A 111.1 . . ? O5 C27 H27B 111.1 . . ? C26 C27 H27B 111.1 . . ? H27A C27 H27B 109.0 . . ? N6 C28 O6 118.5(5) . . ? N6 C28 C20 126.4(5) . . ? O6 C28 C20 115.1(5) . . ? N6 C29 C30 104.2(5) . . ? N6 C29 H29A 110.9 . . ? C30 C29 H29A 110.9 . . ? N6 C29 H29B 110.9 . . ? C30 C29 H29B 110.9 . . ? H29A C29 H29B 108.9 . . ? O6 C30 C29 104.7(5) . . ? O6 C30 H30A 110.8 . . ? C29 C30 H30A 110.8 . . ? O6 C30 H30B 110.8 . . ? C29 C30 H30B 110.8 . . ? H30A C30 H30B 108.9 . . ? C32 C31 C36 119.8(5) . . ? C32 C31 C37 121.9(5) . . ? C36 C31 C37 118.3(5) . . ? C31 C32 C33 120.2(5) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 119.2(5) . . ? C34 C33 C40 119.2(5) . . ? C32 C33 C40 121.6(5) . . ? C35 C34 C33 120.4(5) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C36 C35 C34 120.4(5) . . ? C36 C35 C43 120.4(6) . . ? C34 C35 C43 119.2(5) . . ? C35 C36 C31 119.9(5) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? N7 C37 O7 117.0(5) . . ? N7 C37 C31 127.3(5) . . ? O7 C37 C31 115.7(5) . . ? N7 C38 C39 103.8(5) . . ? N7 C38 H38A 111.0 . . ? C39 C38 H38A 111.0 . . ? N7 C38 H38B 111.0 . . ? C39 C38 H38B 111.0 . . ? H38A C38 H38B 109.0 . . ? O7 C39 C38 104.4(5) . . ? O7 C39 H39A 110.9 . . ? C38 C39 H39A 110.9 . . ? O7 C39 H39B 110.9 . . ? C38 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? N8 C40 O8 117.1(6) . . ? N8 C40 C33 127.9(5) . . ? O8 C40 C33 115.0(5) . . ? N8 C41 C42 103.7(6) . . ? N8 C41 H41A 111.0 . . ? C42 C41 H41A 111.0 . . ? N8 C41 H41B 111.0 . . ? C42 C41 H41B 111.0 . . ? H41A C41 H41B 109.0 . . ? O8 C42 C41 105.2(5) . . ? O8 C42 H42A 110.7 . . ? C41 C42 H42A 110.7 . . ? O8 C42 H42B 110.7 . . ? C41 C42 H42B 110.7 . . ? H42A C42 H42B 108.8 . . ? N9 C43 O9 118.2(5) . . ? N9 C43 C35 126.0(5) . . ? O9 C43 C35 115.8(5) . . ? C45 C44 N9 104.2(5) . . ? C45 C44 H44A 110.9 . . ? N9 C44 H44A 110.9 . . ? C45 C44 H44B 110.9 . . ? N9 C44 H44B 110.9 . . ? H44A C44 H44B 108.9 . . ? O9 C45 C44 105.4(5) . . ? O9 C45 H45A 110.7 . . ? C44 C45 H45A 110.7 . . ? O9 C45 H45B 110.7 . . ? C44 C45 H45B 110.7 . . ? H45A C45 H45B 108.8 . . ? C47 C46 C51 120.2(5) . . ? C47 C46 C52 119.9(5) . . ? C51 C46 C52 119.9(5) . . ? C46 C47 C48 120.6(5) . . ? C46 C47 H47A 119.7 . . ? C48 C47 H47A 119.7 . . ? C49 C48 C47 119.3(5) . . ? C49 C48 C55 122.1(5) . . ? C47 C48 C55 118.6(5) . . ? C50 C49 C48 119.4(5) . . ? C50 C49 H49A 120.3 . . ? C48 C49 H49A 120.3 . . ? C51 C50 C49 121.0(5) . . ? C51 C50 C58 119.2(4) . . ? C49 C50 C58 119.8(5) . . ? C50 C51 C46 119.4(5) . . ? C50 C51 H51A 120.3 . . ? C46 C51 H51A 120.3 . . ? N10 C52 O10 118.3(5) . . ? N10 C52 C46 126.1(5) . . ? O10 C52 C46 115.6(5) . . ? N10 C53 C54 104.6(5) . . ? N10 C53 H53A 110.8 . . ? C54 C53 H53A 110.8 . . ? N10 C53 H53B 110.8 . . ? C54 C53 H53B 110.8 . . ? H53A C53 H53B 108.9 . . ? O10 C54 C53 103.0(5) . . ? O10 C54 H54A 111.2 . . ? C53 C54 H54A 111.2 . . ? O10 C54 H54B 111.2 . . ? C53 C54 H54B 111.2 . . ? H54A C54 H54B 109.1 . . ? N11 C55 O11 118.0(5) . . ? N11 C55 C48 128.2(5) . . ? O11 C55 C48 113.8(5) . . ? O11 C56 C57 104.0(5) . . ? O11 C56 H56A 111.0 . . ? C57 C56 H56A 111.0 . . ? O11 C56 H56B 111.0 . . ? C57 C56 H56B 111.0 . . ? H56A C56 H56B 109.0 . . ? C56 C57 N11 105.2(5) . . ? C56 C57 H57A 110.7 . . ? N11 C57 H57A 110.7 . . ? C56 C57 H57B 110.7 . . ? N11 C57 H57B 110.7 . . ? H57A C57 H57B 108.8 . . ? N12 C58 O12 118.9(5) . . ? N12 C58 C50 126.7(4) . . ? O12 C58 C50 114.5(4) . . ? N12 C59 C60 104.1(4) . . ? N12 C59 H59A 110.9 . . ? C60 C59 H59A 110.9 . . ? N12 C59 H59B 110.9 . . ? C60 C59 H59B 110.9 . . ? H59A C59 H59B 109.0 . . ? O12 C60 C59 103.9(5) . . ? O12 C60 H60A 111.0 . . ? C59 C60 H60A 111.0 . . ? O12 C60 H60B 111.0 . . ? C59 C60 H60B 111.0 . . ? H60A C60 H60B 109.0 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.798 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.094 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 765871' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Cu3(OX1)2(MeCN)3](ClO4)3 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H39 Cl3 Cu3 N9 O18' _chemical_formula_weight 1182.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c' _symmetry_space_group_name_Hall 'R 3 -2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 23.752(2) _cell_length_b 23.752 _cell_length_c 14.2281(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6951.3(8) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1771 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 19.39 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 1.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5855 _exptl_absorpt_correction_T_max 0.9090 _exptl_absorpt_process_details 'SADABS(Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12129 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2856 _reflns_number_gt 1628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0039P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 2856 _refine_ls_number_parameters 209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.51958(4) 0.15322(4) 0.99726(7) 0.0563(3) Uani 1 1 d . . . Cl1 Cl 0.54618(12) 0.04249(12) 1.16768(17) 0.0691(6) Uani 1 1 d . . . C1 C 0.7152(3) 0.3180(3) 0.8762(4) 0.0396(16) Uani 1 1 d . . . H1A H 0.7481 0.3075 0.8761 0.048 Uiso 1 1 calc R . . C2 C 0.6510(3) 0.2688(3) 0.8763(5) 0.0397(17) Uani 1 1 d . . . C3 C 0.6354(4) 0.2008(4) 0.8803(5) 0.0480(19) Uani 1 1 d . . . C4 C 0.6512(5) 0.1184(4) 0.8430(8) 0.088(3) Uani 1 1 d . . . H4A H 0.6842 0.1109 0.8707 0.106 Uiso 1 1 calc R . . H4B H 0.6380 0.0960 0.7831 0.106 Uiso 1 1 calc R . . C5 C 0.5934(4) 0.0956(4) 0.9082(6) 0.064(2) Uani 1 1 d . . . H5A H 0.5541 0.0617 0.8790 0.076 Uiso 1 1 calc R . . H5B H 0.6006 0.0794 0.9668 0.076 Uiso 1 1 calc R . . C6 C 0.6379(3) 0.2672(3) 1.1260(4) 0.0366(15) Uani 1 1 d . . . H6A H 0.6185 0.2221 1.1281 0.044 Uiso 1 1 calc R . . C7 C 0.5995(3) 0.2949(3) 1.1245(4) 0.0351(15) Uani 1 1 d . . . C8 C 0.5286(4) 0.2553(3) 1.1220(6) 0.048(2) Uani 1 1 d . . . C9 C 0.4289(4) 0.2391(4) 1.1460(9) 0.107(4) Uani 1 1 d . . . H9A H 0.4113 0.2602 1.1073 0.128 Uiso 1 1 calc R . . H9B H 0.4049 0.2257 1.2046 0.128 Uiso 1 1 calc R . . C10 C 0.4256(4) 0.1817(4) 1.0953(8) 0.077(3) Uani 1 1 d . . . H10A H 0.4033 0.1425 1.1331 0.093 Uiso 1 1 calc R . . H10B H 0.4033 0.1743 1.0356 0.093 Uiso 1 1 calc R . . C11 C 0.3950(4) 0.0585(4) 0.8816(7) 0.061(2) Uani 1 1 d . . . C12 C 0.3440(4) 0.0254(5) 0.8138(8) 0.073(3) Uani 1 1 d . . . H12A H 0.3196 -0.0200 0.8290 0.110 Uiso 1 1 calc R . . H12B H 0.3626 0.0307 0.7523 0.110 Uiso 1 1 calc R . . H12C H 0.3157 0.0434 0.8147 0.110 Uiso 1 1 calc R . . O1 O 0.6752(3) 0.1872(3) 0.8312(4) 0.0677(15) Uani 1 1 d . . . O2 O 0.4970(3) 0.2816(3) 1.1628(5) 0.076(2) Uani 1 1 d . . . O3 O 0.5093(5) -0.0042(4) 1.2269(7) 0.148(4) Uani 1 1 d . . . O4 O 0.5090(4) 0.0540(4) 1.1057(8) 0.150(3) Uani 1 1 d . . . O5 O 0.5812(5) 0.0996(5) 1.2129(7) 0.173(4) Uani 1 1 d . . . O6 O 0.5885(4) 0.0277(4) 1.1211(5) 0.133(3) Uani 1 1 d . . . N1 N 0.5889(3) 0.1552(3) 0.9241(4) 0.0481(15) Uani 1 1 d . . . N2 N 0.4948(3) 0.2008(3) 1.0812(5) 0.0468(15) Uani 1 1 d . . . N3 N 0.4334(3) 0.0845(4) 0.9360(6) 0.081(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0501(6) 0.0579(6) 0.0551(6) -0.0034(5) 0.0029(5) 0.0227(5) Cl1 0.0735(15) 0.0708(16) 0.0570(14) 0.0049(12) 0.0064(13) 0.0314(14) C1 0.054(5) 0.056(5) 0.015(4) -0.004(3) -0.007(3) 0.033(4) C2 0.054(5) 0.052(5) 0.018(4) -0.005(3) 0.001(3) 0.031(4) C3 0.053(5) 0.056(5) 0.041(5) -0.008(4) -0.015(4) 0.032(4) C4 0.082(7) 0.064(6) 0.132(10) -0.009(6) 0.028(6) 0.046(6) C5 0.086(6) 0.046(5) 0.058(6) 0.002(4) 0.001(5) 0.032(5) C6 0.042(4) 0.029(4) 0.029(4) -0.001(3) -0.001(3) 0.011(3) C7 0.038(4) 0.046(4) 0.017(4) -0.006(3) -0.004(3) 0.018(4) C8 0.059(5) 0.047(5) 0.050(5) 0.017(4) 0.020(4) 0.035(4) C9 0.043(6) 0.062(6) 0.202(13) -0.015(7) 0.015(7) 0.017(5) C10 0.035(5) 0.061(6) 0.123(9) -0.010(5) 0.006(5) 0.014(4) C11 0.058(6) 0.061(5) 0.060(6) 0.002(5) 0.004(5) 0.026(5) C12 0.052(5) 0.080(6) 0.080(8) -0.024(6) -0.007(5) 0.027(5) O1 0.073(4) 0.069(4) 0.077(4) 0.008(3) 0.022(3) 0.047(3) O2 0.055(4) 0.055(4) 0.129(7) -0.003(3) 0.024(3) 0.035(3) O3 0.188(8) 0.085(5) 0.157(9) 0.056(6) 0.076(7) 0.058(5) O4 0.121(7) 0.194(9) 0.164(9) 0.042(7) -0.003(6) 0.101(7) O5 0.169(9) 0.106(7) 0.161(10) -0.028(7) 0.024(7) 0.008(6) O6 0.185(8) 0.207(8) 0.083(6) 0.036(6) 0.040(5) 0.155(7) N1 0.051(4) 0.042(4) 0.041(4) 0.000(3) -0.006(3) 0.016(3) N2 0.039(3) 0.034(3) 0.062(4) 0.002(3) 0.001(3) 0.014(3) N3 0.052(4) 0.096(6) 0.083(7) -0.025(5) -0.019(4) 0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.927(6) . ? Cu1 N1 1.929(6) . ? Cu1 N3 2.068(8) . ? Cl1 O3 1.317(8) . ? Cl1 O5 1.349(9) . ? Cl1 O4 1.369(8) . ? Cl1 O6 1.388(7) . ? C1 C2 1.377(8) 2_655 ? C1 C2 1.381(8) . ? C1 H1A 0.9300 . ? C2 C1 1.377(8) 3_665 ? C2 C3 1.465(9) . ? C3 N1 1.258(9) . ? C3 O1 1.339(9) . ? C4 O1 1.446(9) . ? C4 C5 1.515(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.488(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.365(8) . ? C6 C7 1.386(8) 2_655 ? C6 H6A 0.9300 . ? C7 C6 1.386(8) 3_665 ? C7 C8 1.463(9) . ? C8 N2 1.273(9) . ? C8 O2 1.325(8) . ? C9 O2 1.436(9) . ? C9 C10 1.509(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.484(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N3 1.118(9) . ? C11 C12 1.436(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N1 145.8(2) . . ? N2 Cu1 N3 104.6(3) . . ? N1 Cu1 N3 106.7(3) . . ? O3 Cl1 O5 111.0(7) . . ? O3 Cl1 O4 110.9(6) . . ? O5 Cl1 O4 104.0(7) . . ? O3 Cl1 O6 110.7(5) . . ? O5 Cl1 O6 108.8(6) . . ? O4 Cl1 O6 111.3(6) . . ? C2 C1 C2 121.0(7) 2_655 . ? C2 C1 H1A 119.5 2_655 . ? C2 C1 H1A 119.5 . . ? C1 C2 C1 119.0(7) 3_665 . ? C1 C2 C3 121.1(7) 3_665 . ? C1 C2 C3 119.8(7) . . ? N1 C3 O1 118.2(7) . . ? N1 C3 C2 126.7(7) . . ? O1 C3 C2 115.1(7) . . ? O1 C4 C5 104.5(6) . . ? O1 C4 H4A 110.9 . . ? C5 C4 H4A 110.9 . . ? O1 C4 H4B 110.9 . . ? C5 C4 H4B 110.9 . . ? H4A C4 H4B 108.9 . . ? N1 C5 C4 103.6(6) . . ? N1 C5 H5A 111.0 . . ? C4 C5 H5A 111.0 . . ? N1 C5 H5B 111.0 . . ? C4 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C7 121.5(7) . 2_655 ? C7 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 2_655 . ? C6 C7 C6 118.5(7) . 3_665 ? C6 C7 C8 121.6(6) . . ? C6 C7 C8 120.0(6) 3_665 . ? N2 C8 O2 117.5(7) . . ? N2 C8 C7 127.0(6) . . ? O2 C8 C7 115.4(7) . . ? O2 C9 C10 104.3(7) . . ? O2 C9 H9A 110.9 . . ? C10 C9 H9A 110.9 . . ? O2 C9 H9B 110.9 . . ? C10 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? N2 C10 C9 103.8(6) . . ? N2 C10 H10A 111.0 . . ? C9 C10 H10A 111.0 . . ? N2 C10 H10B 111.0 . . ? C9 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? N3 C11 C12 177.9(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 O1 C4 106.5(6) . . ? C8 O2 C9 107.4(7) . . ? C3 N1 C5 107.1(6) . . ? C3 N1 Cu1 131.2(5) . . ? C5 N1 Cu1 121.6(5) . . ? C8 N2 C10 106.7(6) . . ? C8 N2 Cu1 131.1(5) . . ? C10 N2 Cu1 121.4(5) . . ? C11 N3 Cu1 160.2(8) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.534 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.070 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 765872' #TrackingRef 'sunwy.cif' _audit_creation_date 'Tue Apr 10 16:17:47 2007' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Cu2Cl(OX1)2](ClO4)-9/4(H2O)-3/4(CH3CN) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31.50 H36.75 Cl2 Cu2 N6.75 O12.25 ' _chemical_formula_sum 'C31.50 H36.75 Cl2 Cu2 N6.75 O12.25' _chemical_formula_weight 903.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m m n' _symmetry_space_group_name_Hall '-P 2ab 2a' _symmetry_Int_Tables_number 59 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z' 'x, -y+1/2, z' '-x+1/2, -y+1/2, z' '-x, -y, -z' 'x-1/2, -y, -z' '-x, y-1/2, -z' 'x-1/2, y-1/2, -z' _cell_length_a 22.988(11) _cell_length_b 25.016(12) _cell_length_c 13.119(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7545(6) _cell_formula_units_Z 8 _cell_measurement_temperature 200 _cell_measurement_reflns_used 14535 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour greenish-yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 55253 _diffrn_reflns_av_R_equivalents 0.1706 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6987 _reflns_number_gt 3623 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6987 _refine_ls_number_parameters 532 _refine_ls_number_restraints 115 _refine_ls_R_factor_all 0.2272 _refine_ls_R_factor_gt 0.1452 _refine_ls_wR_factor_ref 0.4192 _refine_ls_wR_factor_gt 0.3738 _refine_ls_goodness_of_fit_ref 1.299 _refine_ls_restrained_S_all 1.301 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.06940(7) 0.50051(6) 0.71461(11) 0.0751(6) Uani 1 1 d . . . Cu2 Cu 0.07390(7) 0.49210(6) 1.03825(12) 0.0763(6) Uani 1 1 d . . . Cl1 Cl 0.02777(15) 0.51511(14) 0.8761(2) 0.0765(10) Uani 1 1 d . . . Cl2 Cl 0.0522(3) 0.7500 0.8759(4) 0.0900(16) Uani 1 2 d S . . Cl3 Cl 0.0572(6) 0.7500 0.3776(8) 0.175(4) Uani 1 2 d S . . O1 O 0.0680(4) 0.6357(4) 0.5384(5) 0.075(2) Uani 1 1 d . . . O3 O 0.0805(5) 0.3859(4) 0.4707(7) 0.108(3) Uani 1 1 d . . . O5 O 0.1157(5) 0.6286(4) 0.1980(6) 0.107(3) Uani 1 1 d . . . O11 O 0.2500 0.2500 0.1874(16) 0.103(6) Uani 1 4 d SU . . O12 O 0.2500 0.7500 0.361(6) 0.47(5) Uani 1 4 d SU . . O13 O 0.2500 0.7500 0.210(6) 0.22(3) Uiso 0.70(8) 4 d SPU . . O13B O 0.2500 0.7500 0.114(13) 0.20(5) Uiso 0.30(8) 4 d SPU . . O14 O 0.2500 0.7500 0.624(3) 0.29(2) Uani 1 4 d SU . . O15 O 0.4978(18) 0.2500 0.870(3) 0.31(2) Uani 1 2 d SU . . O16 O 0.2500 0.2500 0.414(7) 0.54(6) Uani 1 4 d SU . . O17 O 0.2500 0.544(2) 0.199(3) 0.326(18) Uani 1 2 d SU . . O21 O 0.0298(13) 0.7500 0.980(2) 0.250(12) Uani 1 2 d SU . . O22 O 0.0059(7) 0.7500 0.8066(14) 0.146(7) Uani 1 2 d SU . . O23 O 0.0825(11) 0.7101(8) 0.8643(15) 0.260(11) Uani 1 1 d U . . O31 O 0.0035(17) 0.7500 0.443(4) 0.325(18) Uani 1 2 d SU . . O32 O 0.1189(12) 0.7500 0.409(3) 0.280(16) Uani 1 2 d SU . . O33 O 0.0471(12) 0.7052(9) 0.3149(19) 0.283(12) Uani 1 1 d U . . O101 O 0.2004(5) 0.5792(5) 0.5137(9) 0.111(4) Uani 0.50 1 d P . . O103 O 0.1476(4) 0.3514(4) 0.7074(7) 0.090(3) Uani 1 1 d . . . O201 O 0.2013(4) 0.5729(4) 0.8268(7) 0.083(3) Uani 0.50 1 d P . . O203 O 0.1447(4) 0.3422(3) 0.9956(8) 0.097(3) Uani 1 1 d . . . N1 N 0.0650(4) 0.5686(4) 0.6467(7) 0.067(3) Uani 1 1 d . . . N3 N 0.0959(5) 0.3794(4) 0.3034(8) 0.083(3) Uani 1 1 d . . . N5 N 0.0993(4) 0.5591(4) 0.0959(6) 0.068(3) Uani 1 1 d . . . N101 N 0.2004(5) 0.5792(5) 0.5137(9) 0.111(4) Uani 0.50 1 d P . . N103 N 0.0961(6) 0.4271(5) 0.7115(7) 0.081(3) Uani 1 1 d . . . N201 N 0.2013(4) 0.5729(4) 0.8268(7) 0.083(3) Uani 0.50 1 d P . . N203 N 0.0970(5) 0.4176(4) 1.0226(7) 0.067(3) Uani 1 1 d . . . N301 N 0.2500 0.2500 0.864(4) 0.34(4) Uani 1 4 d SDU . . N302 N 0.2500 0.4729(17) 0.261(3) 0.30(2) Uani 1 2 d SDU . . C1 C 0.0742(4) 0.5510(5) 0.4624(8) 0.064(3) Uani 1 1 d . . . C2 C 0.0729(5) 0.4960(5) 0.4648(9) 0.066(3) Uani 1 1 d . . . H1 H 0.0644 0.4784 0.5273 0.080 Uiso 1 1 calc R . . C3 C 0.0837(5) 0.4657(6) 0.3787(8) 0.068(3) Uani 1 1 d . . . C4 C 0.0923(5) 0.4925(5) 0.2855(10) 0.071(3) Uani 1 1 d . . . H2 H 0.0978 0.4722 0.2251 0.085 Uiso 1 1 calc R . . C5 C 0.0929(5) 0.5477(6) 0.2798(8) 0.067(3) Uani 1 1 d . . . C6 C 0.0838(5) 0.5776(5) 0.3688(8) 0.067(3) Uani 1 1 d . . . H3 H 0.0842 0.6155 0.3662 0.080 Uiso 1 1 calc R . . C11 C 0.0700(5) 0.5841(5) 0.5541(8) 0.060(3) Uani 1 1 d . . . C12 C 0.0609(6) 0.6165(5) 0.7100(9) 0.077(4) Uani 1 1 d . . . H4 H 0.0903 0.6157 0.7651 0.092 Uiso 1 1 calc R . . H5 H 0.0217 0.6195 0.7411 0.092 Uiso 1 1 calc R . . C13 C 0.0722(6) 0.6632(6) 0.6370(9) 0.086(4) Uani 1 1 d . . . H6 H 0.0423 0.6915 0.6438 0.103 Uiso 1 1 calc R . . H7 H 0.1113 0.6789 0.6476 0.103 Uiso 1 1 calc R . . C31 C 0.0852(6) 0.4088(6) 0.3817(10) 0.079(4) Uani 1 1 d . . . C32 C 0.0970(9) 0.3254(7) 0.3328(12) 0.117(6) Uani 1 1 d . . . H8 H 0.1349 0.3088 0.3163 0.140 Uiso 1 1 calc R . . H9 H 0.0656 0.3050 0.2989 0.140 Uiso 1 1 calc R . . C33 C 0.0870(8) 0.3283(6) 0.4535(12) 0.117(6) Uani 1 1 d . . . H10 H 0.0514 0.3086 0.4739 0.140 Uiso 1 1 calc R . . H11 H 0.1207 0.3137 0.4911 0.140 Uiso 1 1 calc R . . C51 C 0.1019(5) 0.5769(5) 0.1858(8) 0.066(3) Uani 1 1 d . . . C52 C 0.1176(7) 0.6026(5) 0.0262(8) 0.086(4) Uani 1 1 d . . . H12 H 0.0890 0.6079 -0.0294 0.103 Uiso 1 1 calc R . . H13 H 0.1564 0.5954 -0.0036 0.103 Uiso 1 1 calc R . . C53 C 0.1191(11) 0.6518(6) 0.1006(8) 0.140(8) Uani 1 1 d . . . H14 H 0.1557 0.6723 0.0925 0.168 Uiso 1 1 calc R . . H15 H 0.0857 0.6760 0.0882 0.168 Uiso 1 1 calc R . . C101 C 0.2500 0.5047(8) 0.5929(14) 0.080(6) Uani 1 2 d S . . C102 C 0.1970(6) 0.4801(6) 0.6239(8) 0.072(3) Uani 1 1 d . . . H16 H 0.1611 0.4980 0.6133 0.086 Uiso 1 1 calc R . . C103 C 0.1976(5) 0.4328(5) 0.6667(8) 0.066(3) Uani 1 1 d . . . C104 C 0.2500 0.4058(8) 0.6890(12) 0.071(5) Uani 1 2 d S . . H17 H 0.2500 0.3710 0.7177 0.086 Uiso 1 2 calc SR . . C111 C 0.2500 0.5577(8) 0.5383(14) 0.091(6) Uani 1 2 d S . . C112 C 0.2152(7) 0.6272(6) 0.4590(14) 0.123(6) Uani 1 1 d . . . H18 H 0.1997 0.6593 0.4941 0.147 Uiso 1 1 calc R . . H19 H 0.1997 0.6262 0.3886 0.147 Uiso 1 1 calc R . . C131 C 0.1448(6) 0.4047(7) 0.6972(8) 0.079(4) Uani 1 1 d . . . C132 C 0.0525(7) 0.3830(6) 0.7348(12) 0.098(5) Uani 1 1 d . . . H20 H 0.0328 0.3894 0.8008 0.118 Uiso 1 1 calc R . . H21 H 0.0227 0.3804 0.6804 0.118 Uiso 1 1 calc R . . C133 C 0.0892(7) 0.3334(7) 0.7388(11) 0.099(5) Uani 1 1 d . . . H22 H 0.0901 0.3184 0.8087 0.118 Uiso 1 1 calc R . . H23 H 0.0741 0.3058 0.6916 0.118 Uiso 1 1 calc R . . C201 C 0.2500 0.4968(8) 0.8983(11) 0.072(5) Uani 1 2 d S . . C202 C 0.1978(5) 0.4706(5) 0.9214(8) 0.069(3) Uani 1 1 d . . . H24 H 0.1619 0.4875 0.9054 0.083 Uiso 1 1 calc R . . C203 C 0.1971(6) 0.4227(5) 0.9650(9) 0.070(3) Uani 1 1 d . . . C204 C 0.2500 0.3983(8) 0.9900(15) 0.094(6) Uani 1 2 d S . . H25 H 0.2500 0.3648 1.0241 0.112 Uiso 1 2 calc SR . . C211 C 0.2500 0.5505(8) 0.8485(14) 0.084(6) Uani 1 2 d S . . C212 C 0.2174(6) 0.6226(6) 0.7768(10) 0.100(5) Uani 1 1 d . . . H26 H 0.2021 0.6538 0.8149 0.120 Uiso 1 1 calc R . . H27 H 0.2021 0.6238 0.7063 0.120 Uiso 1 1 calc R . . C231 C 0.1421(7) 0.3962(5) 0.9969(9) 0.074(3) Uani 1 1 d . . . C232 C 0.0543(6) 0.3749(5) 1.0459(10) 0.083(4) Uani 1 1 d . . . H28 H 0.0223 0.3747 0.9953 0.099 Uiso 1 1 calc R . . H29 H 0.0376 0.3797 1.1148 0.099 Uiso 1 1 calc R . . C233 C 0.0893(7) 0.3240(6) 1.0398(12) 0.096(4) Uani 1 1 d . . . H30 H 0.0953 0.3083 1.1083 0.116 Uiso 1 1 calc R . . H31 H 0.0701 0.2973 0.9954 0.116 Uiso 1 1 calc R . . C301 C 0.2500 0.2500 0.778(4) 0.35(5) Uani 1 4 d SDU . . C302 C 0.2500 0.2500 0.661(4) 0.20(2) Uani 1 4 d SDU . . H32 H 0.2613 0.2854 0.6357 0.242 Uiso 0.25 1 calc PR . . H33 H 0.2109 0.2413 0.6357 0.242 Uiso 0.25 1 calc PR . . H34 H 0.2777 0.2233 0.6357 0.242 Uiso 0.25 1 calc PR . . C303 C 0.2500 0.4330(18) 0.304(3) 0.31(3) Uani 1 2 d SDU . . C304 C 0.2500 0.3892(18) 0.387(3) 0.215(17) Uani 1 2 d SDU . . H35 H 0.2251 0.4003 0.4434 0.257 Uiso 0.50 1 calc PR . . H36 H 0.2898 0.3836 0.4113 0.257 Uiso 0.50 1 calc PR . . H37 H 0.2351 0.3557 0.3577 0.257 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0847(12) 0.0929(13) 0.0477(9) 0.0062(7) 0.0068(7) 0.0025(9) Cu2 0.0986(13) 0.0772(12) 0.0531(10) -0.0008(7) 0.0101(8) -0.0025(9) Cl1 0.084(2) 0.101(3) 0.0442(16) 0.0029(15) 0.0120(14) 0.0006(18) Cl2 0.124(5) 0.081(4) 0.065(3) 0.000 0.001(3) 0.000 Cl3 0.230(12) 0.134(8) 0.162(8) 0.000 0.019(8) 0.000 O1 0.093(7) 0.089(6) 0.043(4) -0.002(4) 0.000(4) 0.006(5) O3 0.151(10) 0.108(8) 0.065(6) 0.006(6) -0.016(6) -0.011(7) O5 0.180(11) 0.086(7) 0.054(5) -0.009(5) 0.012(6) -0.034(7) O11 0.093(14) 0.103(14) 0.113(15) 0.000 0.000 0.000 O12 0.45(6) 0.51(6) 0.45(6) 0.000 0.000 0.000 O14 0.38(5) 0.29(4) 0.19(3) 0.000 0.000 0.000 O15 0.32(4) 0.35(4) 0.27(3) 0.000 -0.04(3) 0.000 O16 0.47(7) 0.56(7) 0.59(7) 0.000 0.000 0.000 O17 0.24(3) 0.47(4) 0.26(3) -0.11(3) 0.000 0.000 O21 0.22(2) 0.35(3) 0.18(2) 0.000 -0.056(19) 0.000 O22 0.099(12) 0.23(2) 0.111(12) 0.000 -0.030(10) 0.000 O23 0.31(2) 0.227(19) 0.239(19) -0.107(14) -0.079(15) 0.142(16) O31 0.27(3) 0.27(3) 0.44(4) 0.000 0.14(3) 0.000 O32 0.116(18) 0.30(3) 0.42(4) 0.000 -0.04(2) 0.000 O33 0.35(3) 0.25(2) 0.25(2) -0.096(18) 0.01(2) -0.099(19) O101 0.079(8) 0.117(9) 0.136(10) 0.051(8) -0.016(7) 0.000(7) O103 0.092(7) 0.060(6) 0.118(8) 0.017(5) 0.000(6) -0.005(5) O201 0.084(8) 0.081(7) 0.083(6) 0.023(5) 0.008(6) 0.010(6) O203 0.101(8) 0.064(6) 0.126(8) -0.003(5) 0.029(6) -0.014(5) N1 0.074(7) 0.083(7) 0.044(5) -0.003(5) 0.003(4) 0.007(5) N3 0.117(9) 0.066(7) 0.066(7) -0.004(6) 0.003(6) -0.005(6) N5 0.091(8) 0.073(7) 0.041(5) 0.000(5) 0.001(5) -0.001(6) N101 0.079(8) 0.117(9) 0.136(10) 0.051(8) -0.016(7) 0.000(7) N103 0.095(9) 0.107(9) 0.042(5) 0.014(5) 0.002(6) -0.015(7) N201 0.084(8) 0.081(7) 0.083(6) 0.023(5) 0.008(6) 0.010(6) N203 0.072(7) 0.081(7) 0.047(5) -0.001(5) 0.011(5) 0.002(6) N301 0.39(6) 0.26(5) 0.38(6) 0.000 0.000 0.000 N302 0.25(4) 0.29(4) 0.38(4) -0.07(4) 0.000 0.000 C1 0.038(7) 0.095(10) 0.059(7) 0.000(7) 0.007(5) -0.008(6) C2 0.060(8) 0.096(10) 0.042(7) 0.009(6) 0.007(5) -0.016(7) C3 0.078(9) 0.080(10) 0.048(7) -0.007(6) -0.006(6) -0.020(7) C4 0.078(9) 0.073(9) 0.062(8) -0.009(6) 0.004(6) -0.008(7) C5 0.058(8) 0.094(10) 0.051(7) -0.006(7) 0.005(5) -0.018(7) C6 0.072(9) 0.073(8) 0.056(7) 0.001(6) 0.001(6) -0.012(6) C11 0.073(8) 0.062(8) 0.045(6) 0.001(6) 0.000(5) -0.003(6) C12 0.076(9) 0.100(10) 0.054(7) 0.005(7) -0.002(6) -0.005(7) C13 0.102(11) 0.095(11) 0.060(8) -0.007(7) 0.012(7) 0.009(8) C31 0.089(10) 0.095(11) 0.053(8) 0.013(8) -0.025(7) -0.016(8) C32 0.147(16) 0.101(13) 0.103(12) 0.012(10) -0.043(11) -0.014(11) C33 0.172(17) 0.088(12) 0.090(11) 0.004(9) -0.014(11) 0.018(11) C51 0.083(9) 0.071(9) 0.045(7) -0.004(6) 0.005(6) -0.002(7) C52 0.135(13) 0.077(9) 0.045(6) 0.016(6) 0.009(7) -0.012(8) C53 0.28(3) 0.111(12) 0.031(7) 0.011(7) 0.003(10) -0.069(14) C101 0.092(16) 0.098(15) 0.051(10) -0.009(10) 0.000 0.000 C102 0.073(9) 0.088(10) 0.054(7) -0.001(7) -0.017(6) 0.006(7) C103 0.069(9) 0.081(10) 0.048(6) -0.013(6) -0.001(6) -0.003(7) C104 0.072(13) 0.092(13) 0.049(9) -0.021(9) 0.000 0.000 C111 0.12(2) 0.086(15) 0.067(12) 0.003(11) 0.000 0.000 C112 0.126(13) 0.102(12) 0.139(15) 0.033(11) -0.019(10) -0.019(9) C131 0.044(8) 0.151(15) 0.042(6) 0.001(8) -0.005(6) 0.005(9) C132 0.083(11) 0.118(13) 0.094(10) 0.031(9) 0.010(8) 0.002(10) C133 0.096(12) 0.115(13) 0.085(10) 0.013(9) 0.004(8) -0.024(10) C201 0.066(13) 0.120(17) 0.031(8) -0.019(9) 0.000 0.000 C202 0.069(9) 0.082(9) 0.058(7) -0.009(7) 0.006(6) 0.024(7) C203 0.083(10) 0.062(8) 0.064(7) -0.005(6) 0.004(7) 0.000(7) C204 0.12(2) 0.077(14) 0.082(13) -0.009(11) 0.000 0.000 C211 0.112(19) 0.071(14) 0.069(12) 0.008(10) 0.000 0.000 C212 0.098(10) 0.126(13) 0.074(9) 0.023(9) -0.013(7) 0.011(9) C231 0.093(11) 0.076(10) 0.051(7) -0.007(6) 0.005(7) -0.005(8) C232 0.088(10) 0.087(10) 0.073(8) -0.011(7) 0.015(7) -0.025(8) C233 0.117(13) 0.074(10) 0.097(11) 0.007(8) 0.010(9) -0.011(9) C301 0.38(6) 0.34(6) 0.33(6) 0.000 0.000 0.000 C302 0.19(4) 0.11(3) 0.31(5) 0.000 0.000 0.000 C303 0.19(4) 0.37(5) 0.37(5) 0.12(4) 0.000 0.000 C304 0.11(2) 0.32(4) 0.21(3) 0.05(3) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.924(10) . ? Cu1 N103 1.936(12) . ? Cu1 Cl1 2.353(3) . ? Cu2 N5 1.929(10) 1_556 ? Cu2 N203 1.948(11) . ? Cu2 Cl1 2.446(3) . ? Cu2 Cl1 2.599(4) 5_567 ? Cl1 Cu2 2.599(4) 5_567 ? Cl2 O23 1.226(16) . ? Cl2 O23 1.226(17) 3_565 ? Cl2 O22 1.399(16) . ? Cl2 O21 1.46(3) . ? Cl3 O33 1.410(19) 3_565 ? Cl3 O33 1.410(19) . ? Cl3 O32 1.48(3) . ? Cl3 O31 1.50(4) . ? O1 C11 1.308(13) . ? O1 C13 1.468(14) . ? O3 C31 1.304(14) . ? O3 C33 1.468(16) . ? O5 C51 1.341(13) . ? O5 C53 1.406(14) . ? O13 O13B 1.26(13) . ? O101 C111 1.302(13) . ? O101 C112 1.441(16) . ? O103 C131 1.342(17) . ? O103 C133 1.474(16) . ? O201 C211 1.283(12) . ? O201 C212 1.454(15) . ? O203 C231 1.352(14) . ? O203 C233 1.471(16) . ? N1 C11 1.280(13) . ? N1 C12 1.462(15) . ? N3 C31 1.287(16) . ? N3 C32 1.405(17) . ? N5 C51 1.263(13) . ? N5 C52 1.481(13) . ? N5 Cu2 1.929(10) 1_554 ? N103 C131 1.267(16) . ? N103 C132 1.522(18) . ? N203 C231 1.216(15) . ? N203 C232 1.482(16) . ? N301 C301 1.13(7) . ? N302 C303 1.15(6) . ? C1 C2 1.378(15) . ? C1 C6 1.414(15) . ? C1 C11 1.465(16) . ? C2 C3 1.383(16) . ? C2 H1 0.9500 . ? C3 C4 1.408(16) . ? C3 C31 1.424(19) . ? C4 C5 1.383(16) . ? C4 H2 0.9500 . ? C5 C6 1.400(15) . ? C5 C51 1.449(16) . ? C6 H3 0.9500 . ? C12 C13 1.534(17) . ? C12 H4 0.9900 . ? C12 H5 0.9900 . ? C13 H6 0.9900 . ? C13 H7 0.9900 . ? C32 C33 1.60(2) . ? C32 H8 0.9900 . ? C32 H9 0.9900 . ? C33 H10 0.9900 . ? C33 H11 0.9900 . ? C52 C53 1.572(17) . ? C52 H12 0.9900 . ? C52 H13 0.9900 . ? C53 H14 0.9900 . ? C53 H15 0.9900 . ? C101 C102 1.424(16) . ? C101 C102 1.424(16) 2 ? C101 C111 1.51(3) . ? C102 C103 1.308(16) . ? C102 H16 0.9500 . ? C103 C104 1.412(16) . ? C103 C131 1.459(17) . ? C104 C103 1.412(16) 2 ? C104 H17 0.9500 . ? C111 N101 1.302(13) 2 ? C111 O101 1.302(13) 2 ? C112 C112 1.60(3) 2 ? C112 H18 0.9900 . ? C112 H19 0.9900 . ? C132 C133 1.50(2) . ? C132 H20 0.9900 . ? C132 H21 0.9900 . ? C133 H22 0.9900 . ? C133 H23 0.9900 . ? C201 C202 1.401(16) . ? C201 C202 1.401(16) 2 ? C201 C211 1.49(3) . ? C202 C203 1.328(16) . ? C202 H24 0.9500 . ? C203 C204 1.399(15) . ? C203 C231 1.488(18) . ? C204 C203 1.399(15) 2 ? C204 H25 0.9500 . ? C211 N201 1.283(12) 2 ? C211 O201 1.283(12) 2 ? C212 C212 1.50(3) 2 ? C212 H26 0.9900 . ? C212 H27 0.9900 . ? C232 C233 1.508(19) . ? C232 H28 0.9900 . ? C232 H29 0.9900 . ? C233 H30 0.9900 . ? C233 H31 0.9900 . ? C301 C302 1.54(7) . ? C302 H32 0.9800 . ? C302 H33 0.9800 . ? C302 H34 0.9800 . ? C303 C304 1.55(6) . ? C304 H35 0.9800 . ? C304 H36 0.9800 . ? C304 H37 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N103 147.8(4) . . ? N1 Cu1 Cl1 105.0(3) . . ? N103 Cu1 Cl1 107.2(3) . . ? N5 Cu2 N203 142.1(4) 1_556 . ? N5 Cu2 Cl1 105.5(3) 1_556 . ? N203 Cu2 Cl1 104.6(3) . . ? N5 Cu2 Cl1 99.4(3) 1_556 5_567 ? N203 Cu2 Cl1 102.9(3) . 5_567 ? Cl1 Cu2 Cl1 90.13(11) . 5_567 ? Cu1 Cl1 Cu2 124.76(16) . . ? Cu1 Cl1 Cu2 138.07(15) . 5_567 ? Cu2 Cl1 Cu2 89.87(11) . 5_567 ? O23 Cl2 O23 109(3) . 3_565 ? O23 Cl2 O22 110.5(10) . . ? O23 Cl2 O22 110.5(10) 3_565 . ? O23 Cl2 O21 108.5(12) . . ? O23 Cl2 O21 108.5(12) 3_565 . ? O22 Cl2 O21 109.8(13) . . ? O33 Cl3 O33 105(2) 3_565 . ? O33 Cl3 O32 108.8(16) 3_565 . ? O33 Cl3 O32 108.8(16) . . ? O33 Cl3 O31 101.4(18) 3_565 . ? O33 Cl3 O31 101.4(18) . . ? O32 Cl3 O31 129(3) . . ? C11 O1 C13 108.8(9) . . ? C31 O3 C33 106.6(12) . . ? C51 O5 C53 107.6(9) . . ? C111 O101 C112 105.1(13) . . ? C131 O103 C133 106.7(10) . . ? C211 O201 C212 104.5(12) . . ? C231 O203 C233 105.5(10) . . ? C11 N1 C12 107.2(10) . . ? C11 N1 Cu1 134.7(9) . . ? C12 N1 Cu1 117.7(7) . . ? C31 N3 C32 109.5(12) . . ? C51 N5 C52 107.7(10) . . ? C51 N5 Cu2 133.4(9) . 1_554 ? C52 N5 Cu2 118.8(7) . 1_554 ? C131 N103 C132 106.9(13) . . ? C131 N103 Cu1 134.7(11) . . ? C132 N103 Cu1 118.3(10) . . ? C231 N203 C232 107.7(11) . . ? C231 N203 Cu2 133.1(10) . . ? C232 N203 Cu2 119.2(9) . . ? C2 C1 C6 119.6(11) . . ? C2 C1 C11 123.0(11) . . ? C6 C1 C11 117.3(12) . . ? C1 C2 C3 121.6(11) . . ? C1 C2 H1 119.2 . . ? C3 C2 H1 119.2 . . ? C2 C3 C4 118.3(13) . . ? C2 C3 C31 121.9(12) . . ? C4 C3 C31 119.8(11) . . ? C5 C4 C3 121.6(11) . . ? C5 C4 H2 119.2 . . ? C3 C4 H2 119.2 . . ? C4 C5 C6 119.1(11) . . ? C4 C5 C51 123.4(11) . . ? C6 C5 C51 117.5(12) . . ? C5 C6 C1 119.8(13) . . ? C5 C6 H3 120.1 . . ? C1 C6 H3 120.1 . . ? N1 C11 O1 116.5(10) . . ? N1 C11 C1 127.8(11) . . ? O1 C11 C1 115.5(10) . . ? N1 C12 C13 105.0(9) . . ? N1 C12 H4 110.8 . . ? C13 C12 H4 110.8 . . ? N1 C12 H5 110.8 . . ? C13 C12 H5 110.8 . . ? H4 C12 H5 108.8 . . ? O1 C13 C12 100.5(10) . . ? O1 C13 H6 111.7 . . ? C12 C13 H6 111.7 . . ? O1 C13 H7 111.7 . . ? C12 C13 H7 111.7 . . ? H6 C13 H7 109.4 . . ? N3 C31 O3 118.7(14) . . ? N3 C31 C3 123.6(12) . . ? O3 C31 C3 117.5(13) . . ? N3 C32 C33 103.1(12) . . ? N3 C32 H8 111.1 . . ? C33 C32 H8 111.1 . . ? N3 C32 H9 111.1 . . ? C33 C32 H9 111.1 . . ? H8 C32 H9 109.1 . . ? O3 C33 C32 102.1(11) . . ? O3 C33 H10 111.3 . . ? C32 C33 H10 111.3 . . ? O3 C33 H11 111.3 . . ? C32 C33 H11 111.3 . . ? H10 C33 H11 109.2 . . ? N5 C51 O5 117.6(10) . . ? N5 C51 C5 127.6(12) . . ? O5 C51 C5 114.7(10) . . ? N5 C52 C53 101.5(9) . . ? N5 C52 H12 111.5 . . ? C53 C52 H12 111.5 . . ? N5 C52 H13 111.5 . . ? C53 C52 H13 111.5 . . ? H12 C52 H13 109.3 . . ? O5 C53 C52 103.9(11) . . ? O5 C53 H14 111.0 . . ? C52 C53 H14 111.0 . . ? O5 C53 H15 111.0 . . ? C52 C53 H15 111.0 . . ? H14 C53 H15 109.0 . . ? C102 C101 C102 117.5(18) . 2 ? C102 C101 C111 121.1(9) . . ? C102 C101 C111 121.1(9) 2 . ? C103 C102 C101 120.4(14) . . ? C103 C102 H16 119.8 . . ? C101 C102 H16 119.8 . . ? C102 C103 C104 121.9(13) . . ? C102 C103 C131 123.1(13) . . ? C104 C103 C131 115.0(13) . . ? C103 C104 C103 117.2(18) . 2 ? C103 C104 H17 121.4 . . ? C103 C104 H17 121.4 2 . ? O101 C111 N101 122.5(19) . 2 ? O101 C111 O101 122.5(19) . 2 ? O101 C111 C101 118.7(10) . . ? N101 C111 C101 118.7(10) 2 . ? O101 C111 C101 118.7(10) 2 . ? O101 C112 C112 103.7(8) . 2 ? O101 C112 H18 111.0 . . ? C112 C112 H18 111.0 2 . ? O101 C112 H19 111.0 . . ? C112 C112 H19 111.0 2 . ? H18 C112 H19 109.0 . . ? N103 C131 O103 117.9(13) . . ? N103 C131 C103 124.2(15) . . ? O103 C131 C103 117.9(12) . . ? C133 C132 N103 103.6(12) . . ? C133 C132 H20 111.0 . . ? N103 C132 H20 111.0 . . ? C133 C132 H21 111.0 . . ? N103 C132 H21 111.0 . . ? H20 C132 H21 109.0 . . ? O103 C133 C132 104.5(11) . . ? O103 C133 H22 110.9 . . ? C132 C133 H22 110.9 . . ? O103 C133 H23 110.9 . . ? C132 C133 H23 110.9 . . ? H22 C133 H23 108.9 . . ? C202 C201 C202 117.9(18) . 2 ? C202 C201 C211 121.0(9) . . ? C202 C201 C211 121.0(9) 2 . ? C203 C202 C201 121.7(14) . . ? C203 C202 H24 119.2 . . ? C201 C202 H24 119.2 . . ? C202 C203 C204 119.0(14) . . ? C202 C203 C231 122.2(13) . . ? C204 C203 C231 118.5(13) . . ? C203 C204 C203 120.6(19) . 2 ? C203 C204 H25 119.7 . . ? C203 C204 H25 119.7 2 . ? O201 C211 N201 121.4(18) . 2 ? O201 C211 O201 121.4(18) . 2 ? O201 C211 C201 119.3(9) . . ? N201 C211 C201 119.3(9) 2 . ? O201 C211 C201 119.3(9) 2 . ? O201 C212 C212 104.7(6) . 2 ? O201 C212 H26 110.8 . . ? C212 C212 H26 110.8 2 . ? O201 C212 H27 110.8 . . ? C212 C212 H27 110.8 2 . ? H26 C212 H27 108.9 . . ? N203 C231 O203 118.7(12) . . ? N203 C231 C203 127.4(13) . . ? O203 C231 C203 113.9(12) . . ? N203 C232 C233 104.2(11) . . ? N203 C232 H28 110.9 . . ? C233 C232 H28 110.9 . . ? N203 C232 H29 110.9 . . ? C233 C232 H29 110.9 . . ? H28 C232 H29 108.9 . . ? O203 C233 C232 102.7(10) . . ? O203 C233 H30 111.2 . . ? C232 C233 H30 111.2 . . ? O203 C233 H31 111.2 . . ? C232 C233 H31 111.2 . . ? H30 C233 H31 109.1 . . ? N301 C301 C302 180.00(4) . . ? C301 C302 H32 109.5 . . ? C301 C302 H33 109.5 . . ? H32 C302 H33 109.5 . . ? C301 C302 H34 109.5 . . ? H32 C302 H34 109.5 . . ? H33 C302 H34 109.5 . . ? N302 C303 C304 164(5) . . ? C303 C304 H35 109.5 . . ? C303 C304 H36 109.5 . . ? H35 C304 H36 109.5 . . ? C303 C304 H37 109.5 . . ? H35 C304 H37 109.5 . . ? H36 C304 H37 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 Cl1 Cu2 -127.8(3) . . . . ? N103 Cu1 Cl1 Cu2 49.4(4) . . . . ? N1 Cu1 Cl1 Cu2 92.0(4) . . . 5_567 ? N103 Cu1 Cl1 Cu2 -90.8(4) . . . 5_567 ? N5 Cu2 Cl1 Cu1 105.5(4) 1_556 . . . ? N203 Cu2 Cl1 Cu1 -51.3(4) . . . . ? Cl1 Cu2 Cl1 Cu1 -154.7(2) 5_567 . . . ? N5 Cu2 Cl1 Cu2 -99.8(3) 1_556 . . 5_567 ? N203 Cu2 Cl1 Cu2 103.4(3) . . . 5_567 ? Cl1 Cu2 Cl1 Cu2 0.0 5_567 . . 5_567 ? N103 Cu1 N1 C11 20.5(16) . . . . ? Cl1 Cu1 N1 C11 -164.4(11) . . . . ? N103 Cu1 N1 C12 -151.9(9) . . . . ? Cl1 Cu1 N1 C12 23.2(9) . . . . ? N1 Cu1 N103 C131 53.6(15) . . . . ? Cl1 Cu1 N103 C131 -121.4(11) . . . . ? N1 Cu1 N103 C132 -129.4(10) . . . . ? Cl1 Cu1 N103 C132 55.5(9) . . . . ? N5 Cu2 N203 C231 -46.8(14) 1_556 . . . ? Cl1 Cu2 N203 C231 95.0(12) . . . . ? Cl1 Cu2 N203 C231 -171.5(11) 5_567 . . . ? N5 Cu2 N203 C232 132.4(9) 1_556 . . . ? Cl1 Cu2 N203 C232 -85.9(8) . . . . ? Cl1 Cu2 N203 C232 7.7(9) 5_567 . . . ? C6 C1 C2 C3 3.3(17) . . . . ? C11 C1 C2 C3 -172.5(10) . . . . ? C1 C2 C3 C4 -4.3(18) . . . . ? C1 C2 C3 C31 176.8(11) . . . . ? C2 C3 C4 C5 3.1(19) . . . . ? C31 C3 C4 C5 -177.9(12) . . . . ? C3 C4 C5 C6 -1.0(19) . . . . ? C3 C4 C5 C51 179.7(11) . . . . ? C4 C5 C6 C1 0.0(18) . . . . ? C51 C5 C6 C1 179.3(11) . . . . ? C2 C1 C6 C5 -1.1(17) . . . . ? C11 C1 C6 C5 174.9(10) . . . . ? C12 N1 C11 O1 -2.4(14) . . . . ? Cu1 N1 C11 O1 -175.4(8) . . . . ? C12 N1 C11 C1 -178.6(11) . . . . ? Cu1 N1 C11 C1 8.5(19) . . . . ? C13 O1 C11 N1 11.3(14) . . . . ? C13 O1 C11 C1 -172.0(9) . . . . ? C2 C1 C11 N1 0.5(19) . . . . ? C6 C1 C11 N1 -175.4(11) . . . . ? C2 C1 C11 O1 -175.7(10) . . . . ? C6 C1 C11 O1 8.5(15) . . . . ? C11 N1 C12 C13 -7.0(13) . . . . ? Cu1 N1 C12 C13 167.4(8) . . . . ? C11 O1 C13 C12 -14.0(12) . . . . ? N1 C12 C13 O1 12.3(12) . . . . ? C32 N3 C31 O3 3.4(19) . . . . ? C32 N3 C31 C3 177.2(13) . . . . ? C33 O3 C31 N3 -2.5(18) . . . . ? C33 O3 C31 C3 -176.7(12) . . . . ? C2 C3 C31 N3 -179.0(13) . . . . ? C4 C3 C31 N3 2(2) . . . . ? C2 C3 C31 O3 -5.1(19) . . . . ? C4 C3 C31 O3 176.0(12) . . . . ? C31 N3 C32 C33 -2.6(17) . . . . ? C31 O3 C33 C32 0.6(15) . . . . ? N3 C32 C33 O3 1.2(16) . . . . ? C52 N5 C51 O5 4.2(16) . . . . ? Cu2 N5 C51 O5 -172.1(9) 1_554 . . . ? C52 N5 C51 C5 -174.3(12) . . . . ? Cu2 N5 C51 C5 9(2) 1_554 . . . ? C53 O5 C51 N5 5.2(19) . . . . ? C53 O5 C51 C5 -176.2(14) . . . . ? C4 C5 C51 N5 15(2) . . . . ? C6 C5 C51 N5 -164.7(12) . . . . ? C4 C5 C51 O5 -163.9(12) . . . . ? C6 C5 C51 O5 16.7(17) . . . . ? C51 N5 C52 C53 -10.4(16) . . . . ? Cu2 N5 C52 C53 166.5(11) 1_554 . . . ? C51 O5 C53 C52 -11.2(19) . . . . ? N5 C52 C53 O5 12.9(18) . . . . ? C102 C101 C102 C103 -9(2) 2 . . . ? C111 C101 C102 C103 176.7(14) . . . . ? C101 C102 C103 C104 3.5(19) . . . . ? C101 C102 C103 C131 -178.0(12) . . . . ? C102 C103 C104 C103 2(2) . . . 2 ? C131 C103 C104 C103 -176.2(9) . . . 2 ? C112 O101 C111 N101 0(3) . . . 2 ? C112 O101 C111 O101 0(3) . . . 2 ? C112 O101 C111 C101 -177.1(15) . . . . ? C102 C101 C111 O101 -4(3) . . . . ? C102 C101 C111 O101 -178.4(15) 2 . . . ? C102 C101 C111 N101 178.5(15) . . . 2 ? C102 C101 C111 N101 4(3) 2 . . 2 ? C102 C101 C111 O101 178.5(15) . . . 2 ? C102 C101 C111 O101 4(3) 2 . . 2 ? C111 O101 C112 C112 0.1(13) . . . 2 ? C132 N103 C131 O103 -1.6(15) . . . . ? Cu1 N103 C131 O103 175.7(8) . . . . ? C132 N103 C131 C103 176.1(11) . . . . ? Cu1 N103 C131 C103 -6.7(18) . . . . ? C133 O103 C131 N103 -2.5(15) . . . . ? C133 O103 C131 C103 179.7(10) . . . . ? C102 C103 C131 N103 -19.9(18) . . . . ? C104 C103 C131 N103 158.7(12) . . . . ? C102 C103 C131 O103 157.7(11) . . . . ? C104 C103 C131 O103 -23.7(15) . . . . ? C131 N103 C132 C133 4.8(14) . . . . ? Cu1 N103 C132 C133 -173.0(9) . . . . ? C131 O103 C133 C132 5.3(14) . . . . ? N103 C132 C133 O103 -6.0(14) . . . . ? C202 C201 C202 C203 1(2) 2 . . . ? C211 C201 C202 C203 179.6(13) . . . . ? C201 C202 C203 C204 1.0(19) . . . . ? C201 C202 C203 C231 175.4(11) . . . . ? C202 C203 C204 C203 -3(3) . . . 2 ? C231 C203 C204 C203 -177.6(11) . . . 2 ? C212 O201 C211 N201 1(2) . . . 2 ? C212 O201 C211 O201 1(2) . . . 2 ? C212 O201 C211 C201 -178.0(14) . . . . ? C202 C201 C211 O201 0(2) . . . . ? C202 C201 C211 O201 178.7(14) 2 . . . ? C202 C201 C211 N201 -178.7(14) . . . 2 ? C202 C201 C211 N201 0(2) 2 . . 2 ? C202 C201 C211 O201 -178.7(14) . . . 2 ? C202 C201 C211 O201 0(2) 2 . . 2 ? C211 O201 C212 C212 -0.4(12) . . . 2 ? C232 N203 C231 O203 -0.5(15) . . . . ? Cu2 N203 C231 O203 178.7(8) . . . . ? C232 N203 C231 C203 179.1(11) . . . . ? Cu2 N203 C231 C203 -2(2) . . . . ? C233 O203 C231 N203 -6.4(16) . . . . ? C233 O203 C231 C203 173.9(11) . . . . ? C202 C203 C231 N203 -28(2) . . . . ? C204 C203 C231 N203 146.1(15) . . . . ? C202 C203 C231 O203 151.4(11) . . . . ? C204 C203 C231 O203 -34.2(17) . . . . ? C231 N203 C232 C233 7.1(14) . . . . ? Cu2 N203 C232 C233 -172.3(8) . . . . ? C231 O203 C233 C232 9.9(14) . . . . ? N203 C232 C233 O203 -10.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.169 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.150 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 765873' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 Cl2 Cu2 N8 O16' _chemical_formula_sum 'C34 H40 Cl2 Cu2 N8 O16' _chemical_formula_weight 1014.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0086(6) _cell_length_b 12.9662(11) _cell_length_c 13.0105(11) _cell_angle_alpha 118.6290(10) _cell_angle_beta 93.0040(10) _cell_angle_gamma 99.6650(10) _cell_volume 1010.92(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2108 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.64 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7593 _exptl_absorpt_correction_T_max 0.9279 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apec CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5092 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3525 _reflns_number_gt 2810 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3525 _refine_ls_number_parameters 310 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.58447(6) 0.47452(4) 0.29589(4) 0.04771(18) Uani 1 1 d . . . Cl1 Cl 0.79531(16) 0.09956(9) 0.30011(10) 0.0672(3) Uani 1 1 d . . . O1 O 0.1896(4) 0.17573(19) 0.0349(2) 0.0518(6) Uani 1 1 d . . . O1W O 0.8608(5) 0.3439(3) 0.1966(3) 0.0713(9) Uani 1 1 d . . . O2 O 0.2159(4) 0.1861(2) -0.3385(2) 0.0564(7) Uani 1 1 d . . . O3 O 0.2739(4) 0.72038(19) 0.21474(19) 0.0533(6) Uani 1 1 d . . . O4 O 0.8908(6) 0.2156(3) 0.3299(3) 0.0961(11) Uani 1 1 d . A . O5 O 0.6824(7) 0.0469(5) 0.1871(4) 0.192(3) Uani 1 1 d . A . O6 O 0.9370(7) 0.0326(3) 0.2857(4) 0.1313(16) Uani 1 1 d . A . O7 O 0.714(6) 0.1020(10) 0.395(3) 0.172(10) Uani 0.72(6) 1 d P A 1 O7' O 0.634(3) 0.123(3) 0.3617(17) 0.075(11) Uani 0.28(6) 1 d P A 2 N1 N 0.3830(4) 0.3306(2) 0.1938(2) 0.0375(6) Uani 1 1 d . . . N2 N 0.3189(4) 0.3579(2) -0.3385(2) 0.0387(6) Uani 1 1 d . . . N3 N 0.2375(4) 0.7350(2) 0.0510(2) 0.0448(7) Uani 1 1 d . . . N4 N 0.6932(5) 0.4617(3) 0.4399(3) 0.0567(8) Uani 1 1 d . . . C1 C 0.2718(4) 0.3564(3) 0.0278(3) 0.0330(7) Uani 1 1 d . . . C2 C 0.2628(4) 0.2984(3) -0.0939(3) 0.0342(7) Uani 1 1 d . . . H2A H 0.2614 0.2165 -0.1360 0.041 Uiso 1 1 calc R . . C3 C 0.2558(4) 0.3633(3) -0.1525(3) 0.0344(7) Uani 1 1 d . . . C4 C 0.2490(4) 0.4835(3) -0.0900(3) 0.0347(7) Uani 1 1 d . . . H4A H 0.2395 0.5260 -0.1301 0.042 Uiso 1 1 calc R . . C5 C 0.2561(4) 0.5412(3) 0.0312(3) 0.0326(7) Uani 1 1 d . . . C6 C 0.2691(4) 0.4772(3) 0.0901(3) 0.0345(7) Uani 1 1 d . . . H6A H 0.2762 0.5157 0.1721 0.041 Uiso 1 1 calc R . . C7 C 0.2880(5) 0.2902(3) 0.0923(3) 0.0369(7) Uani 1 1 d . . . C8 C 0.3439(6) 0.2325(3) 0.2228(3) 0.0533(9) Uani 1 1 d . . . H8A H 0.2617 0.2507 0.2843 0.064 Uiso 1 1 calc R . . H8B H 0.4650 0.2190 0.2488 0.064 Uiso 1 1 calc R . . C9 C 0.2402(7) 0.1254(3) 0.1080(3) 0.0676(12) Uani 1 1 d . . . H9A H 0.3254 0.0701 0.0719 0.081 Uiso 1 1 calc R . . H9B H 0.1236 0.0829 0.1201 0.081 Uiso 1 1 calc R . . C10 C 0.2652(5) 0.3056(3) -0.2805(3) 0.0386(7) Uani 1 1 d . . . C11 C 0.3020(6) 0.2616(3) -0.4637(3) 0.0516(9) Uani 1 1 d . . . H11A H 0.4251 0.2675 -0.4934 0.062 Uiso 1 1 calc R . . H11B H 0.2006 0.2664 -0.5138 0.062 Uiso 1 1 calc R . . C12 C 0.2494(8) 0.1465(3) -0.4594(3) 0.0738(13) Uani 1 1 d . . . H12A H 0.1323 0.0938 -0.5151 0.089 Uiso 1 1 calc R . . H12B H 0.3557 0.1043 -0.4773 0.089 Uiso 1 1 calc R . . C13 C 0.2533(4) 0.6700(3) 0.0966(3) 0.0371(7) Uani 1 1 d . . . C14 C 0.2450(6) 0.8565(3) 0.1492(3) 0.0585(10) Uani 1 1 d . . . H14A H 0.1238 0.8814 0.1433 0.070 Uiso 1 1 calc R . . H14B H 0.3528 0.9143 0.1493 0.070 Uiso 1 1 calc R . . C15 C 0.2743(6) 0.8469(3) 0.2585(3) 0.0609(10) Uani 1 1 d . . . H15A H 0.3980 0.8979 0.3076 0.073 Uiso 1 1 calc R . . H15B H 0.1690 0.8700 0.3045 0.073 Uiso 1 1 calc R . . C16 C 0.7590(5) 0.4421(3) 0.5071(3) 0.0453(8) Uani 1 1 d . . . C17 C 0.8444(7) 0.4160(4) 0.5933(4) 0.0597(11) Uani 1 1 d D . . H1WA H 0.832(6) 0.304(4) 0.126(4) 0.068(15) Uiso 1 1 d . . . H17A H 0.905(5) 0.490(3) 0.659(3) 0.074(13) Uiso 1 1 d D . . H17B H 0.745(6) 0.375(3) 0.612(4) 0.13(2) Uiso 1 1 d D . . H1WB H 0.856(7) 0.296(4) 0.210(4) 0.074(17) Uiso 1 1 d . . . H17C H 0.940(5) 0.372(3) 0.562(4) 0.13(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0509(3) 0.0501(3) 0.0429(3) 0.0261(2) 0.00308(19) 0.0046(2) Cl1 0.0648(6) 0.0477(6) 0.0752(7) 0.0208(5) 0.0050(5) 0.0111(5) O1 0.0750(17) 0.0348(13) 0.0458(14) 0.0237(11) -0.0035(12) 0.0044(11) O1W 0.102(3) 0.063(2) 0.056(2) 0.0346(18) 0.0063(17) 0.0194(18) O2 0.0921(19) 0.0347(13) 0.0344(13) 0.0128(11) 0.0086(12) 0.0086(12) O3 0.0775(18) 0.0365(13) 0.0402(14) 0.0128(11) 0.0076(12) 0.0185(12) O4 0.130(3) 0.063(2) 0.097(2) 0.0406(19) 0.019(2) 0.0198(19) O5 0.119(4) 0.208(5) 0.121(4) -0.009(4) -0.046(3) 0.031(3) O6 0.192(4) 0.103(3) 0.127(3) 0.058(3) 0.030(3) 0.095(3) O7 0.264(18) 0.110(6) 0.185(13) 0.087(7) 0.159(14) 0.065(8) O7' 0.093(17) 0.075(13) 0.080(12) 0.053(8) 0.047(10) 0.018(8) N1 0.0424(15) 0.0394(15) 0.0359(15) 0.0236(13) 0.0020(12) 0.0067(12) N2 0.0447(16) 0.0410(15) 0.0293(14) 0.0174(12) 0.0022(11) 0.0081(12) N3 0.0558(18) 0.0344(15) 0.0499(17) 0.0237(14) 0.0056(13) 0.0158(13) N4 0.060(2) 0.070(2) 0.0491(18) 0.0358(17) 0.0072(15) 0.0156(16) C1 0.0311(16) 0.0361(17) 0.0371(17) 0.0221(14) 0.0047(13) 0.0078(13) C2 0.0339(17) 0.0310(16) 0.0365(17) 0.0166(14) 0.0023(13) 0.0053(13) C3 0.0328(16) 0.0388(17) 0.0330(16) 0.0193(14) 0.0040(13) 0.0064(13) C4 0.0353(17) 0.0380(17) 0.0383(17) 0.0236(15) 0.0065(13) 0.0114(13) C5 0.0275(16) 0.0336(16) 0.0368(17) 0.0165(14) 0.0050(12) 0.0100(12) C6 0.0353(17) 0.0389(18) 0.0298(16) 0.0167(14) 0.0059(13) 0.0105(13) C7 0.0411(18) 0.0372(18) 0.0400(18) 0.0233(15) 0.0114(14) 0.0124(14) C8 0.066(2) 0.052(2) 0.054(2) 0.0376(19) 0.0014(18) 0.0095(18) C9 0.104(3) 0.049(2) 0.060(2) 0.039(2) 0.002(2) 0.009(2) C10 0.0406(18) 0.0370(18) 0.0367(17) 0.0167(15) 0.0030(14) 0.0108(14) C11 0.061(2) 0.054(2) 0.0335(18) 0.0176(17) 0.0098(16) 0.0094(18) C12 0.128(4) 0.052(2) 0.037(2) 0.0156(19) 0.013(2) 0.026(2) C13 0.0326(17) 0.0384(18) 0.0387(18) 0.0172(15) 0.0071(13) 0.0095(13) C14 0.065(2) 0.037(2) 0.067(3) 0.0210(19) -0.001(2) 0.0153(17) C15 0.082(3) 0.0325(19) 0.054(2) 0.0096(17) 0.013(2) 0.0149(18) C16 0.043(2) 0.058(2) 0.0368(18) 0.0242(17) 0.0063(15) 0.0127(16) C17 0.064(3) 0.081(3) 0.042(2) 0.035(2) 0.006(2) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.946(2) . ? Cu1 N2 1.949(3) 2_665 ? Cu1 N4 2.076(3) . ? Cl1 O7 1.381(18) . ? Cl1 O6 1.388(4) . ? Cl1 O4 1.392(3) . ? Cl1 O5 1.410(4) . ? Cl1 O7' 1.41(2) . ? O1 C7 1.333(4) . ? O1 C9 1.447(4) . ? O1W H1WA 0.80(4) . ? O1W H1WB 0.73(4) . ? O2 C10 1.328(4) . ? O2 C12 1.448(4) . ? O3 C13 1.339(4) . ? O3 C15 1.456(4) . ? N1 C7 1.261(4) . ? N1 C8 1.480(4) . ? N2 C10 1.267(4) . ? N2 C11 1.486(4) . ? N2 Cu1 1.949(3) 2_665 ? N3 C13 1.257(4) . ? N3 C14 1.468(4) . ? N4 C16 1.120(4) . ? C1 C6 1.380(4) . ? C1 C2 1.381(4) . ? C1 C7 1.472(4) . ? C2 C3 1.386(4) . ? C2 H2A 0.9300 . ? C3 C4 1.381(4) . ? C3 C10 1.473(4) . ? C4 C5 1.377(4) . ? C4 H4A 0.9300 . ? C5 C6 1.383(4) . ? C5 C13 1.471(4) . ? C6 H6A 0.9300 . ? C8 C9 1.499(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.505(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.492(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.446(5) . ? C17 H17A 0.93(3) . ? C17 H17B 0.92(3) . ? C17 H17C 0.93(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 143.64(11) . 2_665 ? N1 Cu1 N4 108.69(11) . . ? N2 Cu1 N4 105.20(11) 2_665 . ? O7 Cl1 O6 104(2) . . ? O7 Cl1 O4 109.6(5) . . ? O6 Cl1 O4 107.6(3) . . ? O7 Cl1 O5 121.5(19) . . ? O6 Cl1 O5 105.5(3) . . ? O4 Cl1 O5 107.6(3) . . ? O7 Cl1 O7' 35.4(10) . . ? O6 Cl1 O7' 137.7(16) . . ? O4 Cl1 O7' 100.9(13) . . ? O5 Cl1 O7' 94.5(9) . . ? C7 O1 C9 105.6(3) . . ? H1WA O1W H1WB 98(5) . . ? C10 O2 C12 106.9(3) . . ? C13 O3 C15 105.4(3) . . ? C7 N1 C8 106.6(3) . . ? C7 N1 Cu1 133.3(2) . . ? C8 N1 Cu1 119.29(19) . . ? C10 N2 C11 106.5(3) . . ? C10 N2 Cu1 134.1(2) . 2_665 ? C11 N2 Cu1 119.4(2) . 2_665 ? C13 N3 C14 106.6(3) . . ? C16 N4 Cu1 171.1(3) . . ? C6 C1 C2 120.4(3) . . ? C6 C1 C7 119.5(3) . . ? C2 C1 C7 120.1(3) . . ? C1 C2 C3 119.3(3) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C10 120.1(3) . . ? C2 C3 C10 119.9(3) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 C13 120.0(3) . . ? C6 C5 C13 120.8(3) . . ? C1 C6 C5 120.3(3) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? N1 C7 O1 118.2(3) . . ? N1 C7 C1 127.0(3) . . ? O1 C7 C1 114.8(3) . . ? N1 C8 C9 103.5(3) . . ? N1 C8 H8A 111.1 . . ? C9 C8 H8A 111.1 . . ? N1 C8 H8B 111.1 . . ? C9 C8 H8B 111.1 . . ? H8A C8 H8B 109.0 . . ? O1 C9 C8 104.4(3) . . ? O1 C9 H9A 110.9 . . ? C8 C9 H9A 110.9 . . ? O1 C9 H9B 110.9 . . ? C8 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? N2 C10 O2 117.9(3) . . ? N2 C10 C3 126.8(3) . . ? O2 C10 C3 115.2(3) . . ? N2 C11 C12 104.2(3) . . ? N2 C11 H11A 110.9 . . ? C12 C11 H11A 110.9 . . ? N2 C11 H11B 110.9 . . ? C12 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? O2 C12 C11 103.9(3) . . ? O2 C12 H12A 111.0 . . ? C11 C12 H12A 111.0 . . ? O2 C12 H12B 111.0 . . ? C11 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? N3 C13 O3 118.7(3) . . ? N3 C13 C5 125.5(3) . . ? O3 C13 C5 115.8(3) . . ? N3 C14 C15 104.9(3) . . ? N3 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? N3 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.8 . . ? O3 C15 C14 104.4(3) . . ? O3 C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? O3 C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? N4 C16 C17 179.6(4) . . ? C16 C17 H17A 107(2) . . ? C16 C17 H17B 108(4) . . ? H17A C17 H17B 112(2) . . ? C16 C17 H17C 109(3) . . ? H17A C17 H17C 108(2) . . ? H17B C17 H17C 112(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C7 30.1(4) 2_665 . . . ? N4 Cu1 N1 C7 -172.1(3) . . . . ? N2 Cu1 N1 C8 -162.1(2) 2_665 . . . ? N4 Cu1 N1 C8 -4.3(3) . . . . ? N1 Cu1 N4 C16 61(2) . . . . ? N2 Cu1 N4 C16 -131.9(19) 2_665 . . . ? C6 C1 C2 C3 1.5(4) . . . . ? C7 C1 C2 C3 -177.3(3) . . . . ? C1 C2 C3 C4 -2.9(4) . . . . ? C1 C2 C3 C10 174.2(3) . . . . ? C2 C3 C4 C5 2.3(4) . . . . ? C10 C3 C4 C5 -174.7(3) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C3 C4 C5 C13 178.6(3) . . . . ? C2 C1 C6 C5 0.4(4) . . . . ? C7 C1 C6 C5 179.3(3) . . . . ? C4 C5 C6 C1 -1.0(4) . . . . ? C13 C5 C6 C1 -180.0(3) . . . . ? C8 N1 C7 O1 -3.3(4) . . . . ? Cu1 N1 C7 O1 165.6(2) . . . . ? C8 N1 C7 C1 176.5(3) . . . . ? Cu1 N1 C7 C1 -14.6(5) . . . . ? C9 O1 C7 N1 -5.5(4) . . . . ? C9 O1 C7 C1 174.7(3) . . . . ? C6 C1 C7 N1 -34.5(5) . . . . ? C2 C1 C7 N1 144.4(3) . . . . ? C6 C1 C7 O1 145.3(3) . . . . ? C2 C1 C7 O1 -35.8(4) . . . . ? C7 N1 C8 C9 10.2(4) . . . . ? Cu1 N1 C8 C9 -160.6(3) . . . . ? C7 O1 C9 C8 11.4(4) . . . . ? N1 C8 C9 O1 -12.9(4) . . . . ? C11 N2 C10 O2 2.0(4) . . . . ? Cu1 N2 C10 O2 -176.5(2) 2_665 . . . ? C11 N2 C10 C3 -179.7(3) . . . . ? Cu1 N2 C10 C3 1.8(5) 2_665 . . . ? C12 O2 C10 N2 3.0(4) . . . . ? C12 O2 C10 C3 -175.5(3) . . . . ? C4 C3 C10 N2 20.0(5) . . . . ? C2 C3 C10 N2 -157.1(3) . . . . ? C4 C3 C10 O2 -161.7(3) . . . . ? C2 C3 C10 O2 21.2(4) . . . . ? C10 N2 C11 C12 -5.9(4) . . . . ? Cu1 N2 C11 C12 172.9(3) 2_665 . . . ? C10 O2 C12 C11 -6.4(4) . . . . ? N2 C11 C12 O2 7.3(4) . . . . ? C14 N3 C13 O3 -0.6(4) . . . . ? C14 N3 C13 C5 -179.0(3) . . . . ? C15 O3 C13 N3 -0.8(4) . . . . ? C15 O3 C13 C5 177.8(3) . . . . ? C4 C5 C13 N3 2.8(5) . . . . ? C6 C5 C13 N3 -178.3(3) . . . . ? C4 C5 C13 O3 -175.7(3) . . . . ? C6 C5 C13 O3 3.2(4) . . . . ? C13 N3 C14 C15 1.7(4) . . . . ? C13 O3 C15 C14 1.8(4) . . . . ? N3 C14 C15 O3 -2.1(4) . . . . ? Cu1 N4 C16 C17 2(65) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA N3 0.80(4) 2.12(4) 2.876(5) 158(4) 2_665 O1W H1WB O4 0.73(4) 2.27(5) 2.943(5) 155(5) . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.433 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.068 #====END data_5 _database_code_depnum_ccdc_archive 'CCDC 765874' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H15 Br2 Cu2 N3 O3' _chemical_formula_sum 'C15 H15 Br2 Cu2 N3 O3' _chemical_formula_weight 572.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.145(9) _cell_length_b 11.1913(15) _cell_length_c 11.4001(16) _cell_angle_alpha 85.809(3) _cell_angle_beta 76.365(3) _cell_angle_gamma 77.003(3) _cell_volume 863.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 730 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 22.23 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 7.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5669 _exptl_absorpt_correction_T_max 0.8149 _exptl_absorpt_process_details 'sadabs (Bruker 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4347 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2998 _reflns_number_gt 2120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2998 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.77146(14) 0.84430(8) -0.42475(8) 0.0506(3) Uani 1 1 d . . . Br2 Br 0.76457(11) 0.89616(7) -0.06540(7) 0.0368(2) Uani 1 1 d . . . Cu1 Cu 0.60632(15) 0.13695(8) -0.01554(9) 0.0390(3) Uani 1 1 d . . . Cu2 Cu 0.80313(15) 0.76805(9) -0.22894(9) 0.0422(3) Uani 1 1 d . . . O1 O 0.9860(8) 0.3822(4) -0.2152(5) 0.0406(14) Uani 1 1 d . . . O2 O 0.7472(7) 0.2122(4) 0.2977(4) 0.0331(12) Uani 1 1 d . . . O3 O 0.4136(8) 0.6584(5) 0.3352(4) 0.0407(14) Uani 1 1 d . . . N1 N 0.8974(9) 0.5861(6) -0.2317(6) 0.0368(16) Uani 1 1 d . . . N2 N 0.6937(8) 0.1375(5) 0.1347(5) 0.0270(14) Uani 1 1 d . . . N3 N 0.3885(8) 0.7846(5) 0.1740(5) 0.0275(14) Uani 1 1 d . . . C1 C 0.7889(9) 0.4822(6) -0.0388(6) 0.0216(15) Uani 1 1 d . . . C2 C 0.7981(10) 0.3671(6) 0.0180(7) 0.0268(16) Uani 1 1 d . . . H2A H 0.8720 0.2978 -0.0245 0.032 Uiso 1 1 calc R . . C3 C 0.7007(10) 0.3542(6) 0.1349(6) 0.0258(16) Uani 1 1 d . . . C4 C 0.5939(10) 0.4551(6) 0.1995(6) 0.0257(16) Uani 1 1 d . . . H4A H 0.5301 0.4462 0.2797 0.031 Uiso 1 1 calc R . . C5 C 0.5808(10) 0.5713(6) 0.1452(6) 0.0237(16) Uani 1 1 d . . . C6 C 0.6785(10) 0.5846(6) 0.0276(6) 0.0276(17) Uani 1 1 d . . . H6A H 0.6710 0.6624 -0.0082 0.033 Uiso 1 1 calc R . . C7 C 0.8931(10) 0.4909(6) -0.1658(6) 0.0258(16) Uani 1 1 d . . . C8 C 1.0153(13) 0.5431(7) -0.3540(7) 0.047(2) Uani 1 1 d . . . H8A H 0.9358 0.5638 -0.4137 0.057 Uiso 1 1 calc R . . H8B H 1.1295 0.5799 -0.3787 0.057 Uiso 1 1 calc R . . C9 C 1.0766(14) 0.4076(7) -0.3391(7) 0.049(2) Uani 1 1 d . . . H9A H 1.0298 0.3655 -0.3942 0.059 Uiso 1 1 calc R . . H9B H 1.2190 0.3820 -0.3538 0.059 Uiso 1 1 calc R . . C10 C 0.7111(10) 0.2288(6) 0.1874(6) 0.0239(16) Uani 1 1 d . . . C11 C 0.7284(12) 0.0298(7) 0.2158(6) 0.0363(19) Uani 1 1 d . . . H11A H 0.8438 -0.0304 0.1786 0.044 Uiso 1 1 calc R . . H11B H 0.6154 -0.0084 0.2357 0.044 Uiso 1 1 calc R . . C12 C 0.7598(12) 0.0805(6) 0.3269(7) 0.038(2) Uani 1 1 d . . . H12A H 0.6585 0.0683 0.3972 0.045 Uiso 1 1 calc R . . H12B H 0.8879 0.0418 0.3420 0.045 Uiso 1 1 calc R . . C13 C 0.4592(10) 0.6790(6) 0.2149(6) 0.0252(16) Uani 1 1 d . . . C14 C 0.2621(11) 0.8531(7) 0.2802(7) 0.037(2) Uani 1 1 d . . . H14A H 0.1238 0.8593 0.2821 0.045 Uiso 1 1 calc R . . H14B H 0.2864 0.9351 0.2792 0.045 Uiso 1 1 calc R . . C15 C 0.3185(13) 0.7798(7) 0.3863(7) 0.044(2) Uani 1 1 d . . . H15A H 0.4094 0.8143 0.4176 0.053 Uiso 1 1 calc R . . H15B H 0.2034 0.7755 0.4503 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0637(6) 0.0443(5) 0.0368(5) 0.0012(4) -0.0096(4) 0.0004(4) Br2 0.0407(5) 0.0264(4) 0.0407(5) -0.0065(3) -0.0035(4) -0.0058(3) Cu1 0.0543(7) 0.0301(5) 0.0334(6) 0.0001(4) -0.0171(5) -0.0035(5) Cu2 0.0523(7) 0.0336(6) 0.0383(6) -0.0034(5) -0.0050(5) -0.0090(5) O1 0.057(4) 0.026(3) 0.029(3) -0.006(2) 0.004(3) -0.001(3) O2 0.049(3) 0.024(3) 0.028(3) 0.004(2) -0.015(3) -0.006(2) O3 0.055(3) 0.033(3) 0.025(3) -0.002(2) -0.003(3) 0.004(3) N1 0.050(4) 0.028(3) 0.028(4) -0.005(3) -0.001(3) -0.009(3) N2 0.034(3) 0.025(3) 0.026(3) -0.002(3) -0.011(3) -0.007(3) N3 0.033(3) 0.020(3) 0.027(3) 0.002(3) -0.008(3) 0.001(3) C1 0.019(4) 0.023(4) 0.025(4) -0.001(3) -0.007(3) -0.006(3) C2 0.027(4) 0.023(4) 0.033(4) -0.006(3) -0.012(3) -0.003(3) C3 0.029(4) 0.023(4) 0.027(4) -0.002(3) -0.011(3) -0.005(3) C4 0.032(4) 0.025(4) 0.023(4) 0.002(3) -0.010(3) -0.008(3) C5 0.027(4) 0.018(3) 0.026(4) 0.001(3) -0.010(3) -0.003(3) C6 0.034(4) 0.026(4) 0.027(4) 0.007(3) -0.011(3) -0.012(3) C7 0.032(4) 0.021(4) 0.026(4) 0.003(3) -0.009(3) -0.008(3) C8 0.068(6) 0.044(5) 0.023(4) -0.008(4) -0.002(4) -0.005(5) C9 0.066(6) 0.041(5) 0.029(5) -0.004(4) 0.007(4) -0.003(4) C10 0.028(4) 0.022(4) 0.021(4) 0.001(3) -0.004(3) -0.006(3) C11 0.059(5) 0.025(4) 0.027(4) 0.008(3) -0.015(4) -0.009(4) C12 0.054(5) 0.026(4) 0.030(4) 0.009(3) -0.006(4) -0.007(4) C13 0.029(4) 0.031(4) 0.018(4) -0.005(3) -0.004(3) -0.010(3) C14 0.045(5) 0.024(4) 0.036(5) -0.007(4) -0.002(4) 0.002(4) C15 0.054(5) 0.040(5) 0.028(5) -0.017(4) 0.001(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu2 2.3739(14) . ? Br2 Cu2 2.3618(13) . ? Br2 Cu1 2.693(3) 2_665 ? Br2 Cu1 2.7228(13) 1_565 ? Cu1 N3 1.946(6) 2_665 ? Cu1 N2 1.958(6) . ? Cu1 Br2 2.693(3) 2_665 ? Cu1 Br2 2.7228(13) 1_545 ? Cu2 N1 1.996(6) . ? O1 C7 1.341(8) . ? O1 C9 1.444(9) . ? O2 C10 1.333(8) . ? O2 C12 1.474(8) . ? O3 C13 1.348(8) . ? O3 C15 1.470(9) . ? N1 C7 1.260(9) . ? N1 C8 1.499(9) . ? N2 C10 1.265(8) . ? N2 C11 1.476(8) . ? N3 C13 1.277(8) . ? N3 C14 1.476(8) . ? N3 Cu1 1.946(6) 2_665 ? C1 C2 1.394(9) . ? C1 C6 1.395(9) . ? C1 C7 1.471(9) . ? C2 C3 1.364(10) . ? C2 H2A 0.9300 . ? C3 C4 1.368(9) . ? C3 C10 1.478(9) . ? C4 C5 1.392(9) . ? C4 H4A 0.9300 . ? C5 C6 1.372(9) . ? C5 C13 1.478(9) . ? C6 H6A 0.9300 . ? C8 C9 1.490(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.507(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.495(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 Br2 Cu1 89.18(4) . 2_665 ? Cu2 Br2 Cu1 135.62(5) . 1_565 ? Cu1 Br2 Cu1 85.49(5) 2_665 1_565 ? N3 Cu1 N2 144.1(2) 2_665 . ? N3 Cu1 Br2 105.19(17) 2_665 2_665 ? N2 Cu1 Br2 102.19(17) . 2_665 ? N3 Cu1 Br2 103.80(16) 2_665 1_545 ? N2 Cu1 Br2 96.74(17) . 1_545 ? Br2 Cu1 Br2 94.51(5) 2_665 1_545 ? N1 Cu2 Br2 126.48(19) . . ? N1 Cu2 Br1 109.87(19) . . ? Br2 Cu2 Br1 123.24(5) . . ? C7 O1 C9 106.6(5) . . ? C10 O2 C12 105.7(5) . . ? C13 O3 C15 104.7(6) . . ? C7 N1 C8 105.9(6) . . ? C7 N1 Cu2 142.3(5) . . ? C8 N1 Cu2 111.8(5) . . ? C10 N2 C11 106.9(6) . . ? C10 N2 Cu1 128.0(5) . . ? C11 N2 Cu1 124.8(4) . . ? C13 N3 C14 105.5(6) . . ? C13 N3 Cu1 136.3(5) . 2_665 ? C14 N3 Cu1 118.0(4) . 2_665 ? C2 C1 C6 118.2(6) . . ? C2 C1 C7 119.1(6) . . ? C6 C1 C7 122.8(6) . . ? C3 C2 C1 121.2(6) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 120.2(6) . . ? C2 C3 C10 118.1(6) . . ? C4 C3 C10 121.7(6) . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 119.9(6) . . ? C6 C5 C13 120.8(6) . . ? C4 C5 C13 119.3(6) . . ? C5 C6 C1 120.5(6) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? N1 C7 O1 118.3(6) . . ? N1 C7 C1 127.7(7) . . ? O1 C7 C1 114.0(6) . . ? C9 C8 N1 104.7(7) . . ? C9 C8 H8A 110.8 . . ? N1 C8 H8A 110.8 . . ? C9 C8 H8B 110.8 . . ? N1 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? O1 C9 C8 104.5(6) . . ? O1 C9 H9A 110.9 . . ? C8 C9 H9A 110.9 . . ? O1 C9 H9B 110.9 . . ? C8 C9 H9B 110.9 . . ? H9A C9 H9B 108.9 . . ? N2 C10 O2 118.7(6) . . ? N2 C10 C3 125.1(6) . . ? O2 C10 C3 116.2(6) . . ? N2 C11 C12 104.7(6) . . ? N2 C11 H11A 110.8 . . ? C12 C11 H11A 110.8 . . ? N2 C11 H11B 110.8 . . ? C12 C11 H11B 110.8 . . ? H11A C11 H11B 108.9 . . ? O2 C12 C11 103.9(6) . . ? O2 C12 H12A 111.0 . . ? C11 C12 H12A 111.0 . . ? O2 C12 H12B 111.0 . . ? C11 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? N3 C13 O3 118.1(6) . . ? N3 C13 C5 127.7(6) . . ? O3 C13 C5 114.2(6) . . ? N3 C14 C15 104.7(6) . . ? N3 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? N3 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? O3 C15 C14 102.8(6) . . ? O3 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? O3 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 Br2 Cu2 N1 -88.9(2) 2_665 . . . ? Cu1 Br2 Cu2 N1 -171.6(2) 1_565 . . . ? Cu1 Br2 Cu2 Br1 99.18(7) 2_665 . . . ? Cu1 Br2 Cu2 Br1 16.47(10) 1_565 . . . ? Br2 Cu2 N1 C7 34.5(10) . . . . ? Br1 Cu2 N1 C7 -152.7(9) . . . . ? Br2 Cu2 N1 C8 -145.9(5) . . . . ? Br1 Cu2 N1 C8 26.9(6) . . . . ? N3 Cu1 N2 C10 35.2(8) 2_665 . . . ? Br2 Cu1 N2 C10 -103.7(6) 2_665 . . . ? Br2 Cu1 N2 C10 160.1(6) 1_545 . . . ? N3 Cu1 N2 C11 -152.9(5) 2_665 . . . ? Br2 Cu1 N2 C11 68.1(6) 2_665 . . . ? Br2 Cu1 N2 C11 -28.0(6) 1_545 . . . ? C6 C1 C2 C3 0.6(10) . . . . ? C7 C1 C2 C3 -178.7(6) . . . . ? C1 C2 C3 C4 -1.1(10) . . . . ? C1 C2 C3 C10 177.7(6) . . . . ? C2 C3 C4 C5 1.5(10) . . . . ? C10 C3 C4 C5 -177.2(6) . . . . ? C3 C4 C5 C6 -1.4(10) . . . . ? C3 C4 C5 C13 177.9(6) . . . . ? C4 C5 C6 C1 0.9(10) . . . . ? C13 C5 C6 C1 -178.3(6) . . . . ? C2 C1 C6 C5 -0.5(10) . . . . ? C7 C1 C6 C5 178.7(6) . . . . ? C8 N1 C7 O1 -0.1(9) . . . . ? Cu2 N1 C7 O1 179.5(6) . . . . ? C8 N1 C7 C1 -177.2(7) . . . . ? Cu2 N1 C7 C1 2.5(14) . . . . ? C9 O1 C7 N1 1.7(9) . . . . ? C9 O1 C7 C1 179.1(6) . . . . ? C2 C1 C7 N1 178.3(7) . . . . ? C6 C1 C7 N1 -0.9(11) . . . . ? C2 C1 C7 O1 1.2(9) . . . . ? C6 C1 C7 O1 -178.0(6) . . . . ? C7 N1 C8 C9 -1.4(9) . . . . ? Cu2 N1 C8 C9 178.8(6) . . . . ? C7 O1 C9 C8 -2.4(9) . . . . ? N1 C8 C9 O1 2.3(9) . . . . ? C11 N2 C10 O2 -2.1(9) . . . . ? Cu1 N2 C10 O2 170.9(4) . . . . ? C11 N2 C10 C3 175.9(6) . . . . ? Cu1 N2 C10 C3 -11.1(10) . . . . ? C12 O2 C10 N2 0.8(8) . . . . ? C12 O2 C10 C3 -177.3(6) . . . . ? C2 C3 C10 N2 -43.5(10) . . . . ? C4 C3 C10 N2 135.1(8) . . . . ? C2 C3 C10 O2 134.4(7) . . . . ? C4 C3 C10 O2 -46.9(9) . . . . ? C10 N2 C11 C12 2.4(8) . . . . ? Cu1 N2 C11 C12 -170.9(5) . . . . ? C10 O2 C12 C11 0.9(7) . . . . ? N2 C11 C12 O2 -1.9(8) . . . . ? C14 N3 C13 O3 -2.8(9) . . . . ? Cu1 N3 C13 O3 -177.1(5) 2_665 . . . ? C14 N3 C13 C5 174.1(7) . . . . ? Cu1 N3 C13 C5 -0.3(12) 2_665 . . . ? C15 O3 C13 N3 -10.4(9) . . . . ? C15 O3 C13 C5 172.3(6) . . . . ? C6 C5 C13 N3 19.1(11) . . . . ? C4 C5 C13 N3 -160.2(7) . . . . ? C6 C5 C13 O3 -164.0(6) . . . . ? C4 C5 C13 O3 16.8(9) . . . . ? C13 N3 C14 C15 14.5(8) . . . . ? Cu1 N3 C14 C15 -169.9(5) 2_665 . . . ? C13 O3 C15 C14 18.2(8) . . . . ? N3 C14 C15 O3 -19.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.642 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.140 #====END data_6 _database_code_depnum_ccdc_archive 'CCDC 765875' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 Br4 Cu4 N8 O6' _chemical_formula_weight 1226.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnna _symmetry_space_group_name_Hall '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0625(13) _cell_length_b 21.702(2) _cell_length_c 13.4908(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4117.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 5.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3813 _exptl_absorpt_correction_T_max 0.8899 _exptl_absorpt_process_details 'sadabs (Bruker 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19304 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3621 _reflns_number_gt 2683 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+36.2730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3621 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.1028 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.7500 0.0000 -0.23974(14) 0.0358(5) Uani 1 2 d S . . Cu2 Cu 0.42190(11) 0.15374(7) 0.14903(10) 0.0447(4) Uani 1 1 d . . . Br1 Br 0.7500 0.0000 -0.41850(13) 0.0560(6) Uani 1 2 d S . . Br2 Br 0.34248(11) 0.2500 0.2500 0.0397(4) Uani 1 2 d S . . Cu3 Cu 0.5249(2) 0.2500 0.2500 0.0891(10) Uani 1 2 d S . . Br4 Br 0.58030(12) 0.23792(7) 0.09128(16) 0.0885(7) Uani 1 1 d . . . O1 O 0.5776(6) 0.1315(3) -0.1093(6) 0.045(2) Uani 1 1 d . . . O2 O 0.6667(6) -0.1515(3) 0.1410(6) 0.047(2) Uani 1 1 d . . . O3 O 0.5608(6) 0.0271(4) 0.3221(6) 0.048(2) Uani 1 1 d . . . N1 N 0.6710(6) 0.0670(4) -0.1945(7) 0.032(2) Uani 1 1 d . . . N2 N 0.6403(6) -0.1609(4) -0.0210(6) 0.026(2) Uani 1 1 d . . . N3 N 0.4788(6) 0.1008(4) 0.2472(6) 0.032(2) Uani 1 1 d . . . N4 N 0.4306(12) 0.1320(7) 0.6108(12) 0.090(5) Uani 1 1 d . . . C1 C 0.6166(7) 0.0396(4) -0.0249(8) 0.025(2) Uani 1 1 d . . . C2 C 0.6368(7) -0.0223(5) -0.0282(8) 0.029(3) Uani 1 1 d . . . H2A H 0.6559 -0.0400 -0.0878 0.035 Uiso 1 1 calc R . . C3 C 0.6293(7) -0.0589(5) 0.0562(8) 0.030(3) Uani 1 1 d . . . C4 C 0.6003(7) -0.0318(5) 0.1452(8) 0.031(3) Uani 1 1 d . . . H4A H 0.5958 -0.0556 0.2023 0.037 Uiso 1 1 calc R . . C5 C 0.5779(7) 0.0310(5) 0.1490(8) 0.030(2) Uani 1 1 d . . . C6 C 0.5872(7) 0.0666(5) 0.0621(8) 0.030(2) Uani 1 1 d . . . H6A H 0.5733 0.1085 0.0636 0.035 Uiso 1 1 calc R . . C7 C 0.6240(8) 0.0779(5) -0.1149(8) 0.031(3) Uani 1 1 d . . . C8 C 0.6535(9) 0.1192(6) -0.2621(9) 0.050(3) Uani 1 1 d . . . H8A H 0.6144 0.1066 -0.3177 0.061 Uiso 1 1 calc R . . H8B H 0.7129 0.1358 -0.2871 0.061 Uiso 1 1 calc R . . C9 C 0.6021(10) 0.1663(6) -0.1985(10) 0.058(4) Uani 1 1 d . . . H9A H 0.6432 0.2009 -0.1829 0.069 Uiso 1 1 calc R . . H9B H 0.5455 0.1815 -0.2316 0.069 Uiso 1 1 calc R . . C10 C 0.6452(8) -0.1257(5) 0.0525(8) 0.030(3) Uani 1 1 d . . . C11 C 0.6662(9) -0.2239(5) 0.0133(9) 0.041(3) Uani 1 1 d . . . H11A H 0.6196 -0.2540 -0.0083 0.050 Uiso 1 1 calc R . . H11B H 0.7284 -0.2358 -0.0110 0.050 Uiso 1 1 calc R . . C12 C 0.6662(10) -0.2177(5) 0.1231(9) 0.050(3) Uani 1 1 d . . . H12A H 0.6100 -0.2366 0.1515 0.061 Uiso 1 1 calc R . . H12B H 0.7222 -0.2369 0.1515 0.061 Uiso 1 1 calc R . . C13 C 0.5374(8) 0.0561(5) 0.2379(8) 0.031(3) Uani 1 1 d . . . C14 C 0.4561(9) 0.1082(5) 0.3532(8) 0.039(3) Uani 1 1 d . . . H14A H 0.3881 0.1055 0.3644 0.047 Uiso 1 1 calc R . . H14B H 0.4788 0.1475 0.3779 0.047 Uiso 1 1 calc R . . C15 C 0.5075(10) 0.0556(6) 0.4024(9) 0.049(3) Uani 1 1 d . . . H15A H 0.5498 0.0704 0.4539 0.059 Uiso 1 1 calc R . . H15B H 0.4628 0.0266 0.4313 0.059 Uiso 1 1 calc R . . C16 C 0.3538(15) 0.1249(7) 0.6164(12) 0.068(5) Uani 1 1 d . . . C17 C 0.2534(13) 0.1138(9) 0.6279(14) 0.098(6) Uani 1 1 d . . . H17A H 0.2435 0.0721 0.6492 0.146 Uiso 1 1 calc R . . H17B H 0.2219 0.1204 0.5657 0.146 Uiso 1 1 calc R . . H17C H 0.2280 0.1416 0.6766 0.146 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0373(11) 0.0355(11) 0.0346(11) 0.000 0.000 0.0050(9) Cu2 0.0595(10) 0.0420(9) 0.0327(8) 0.0046(7) -0.0070(7) 0.0138(8) Br1 0.0739(14) 0.0620(13) 0.0319(10) 0.000 0.000 -0.0114(11) Br2 0.0380(9) 0.0366(9) 0.0446(10) -0.0114(8) 0.000 0.000 Cu3 0.105(2) 0.0412(16) 0.121(3) -0.0039(16) 0.000 0.000 Br4 0.0672(11) 0.0556(10) 0.1426(18) -0.0242(10) 0.0374(11) -0.0034(8) O1 0.061(6) 0.030(4) 0.043(5) 0.017(4) 0.021(4) 0.016(4) O2 0.079(6) 0.025(4) 0.037(5) -0.002(4) 0.000(4) 0.015(4) O3 0.066(6) 0.049(5) 0.028(5) 0.003(4) -0.005(4) 0.014(4) N1 0.031(5) 0.030(5) 0.034(5) 0.000(4) 0.000(4) 0.012(4) N2 0.040(5) 0.017(4) 0.022(5) 0.000(4) -0.006(4) 0.010(4) N3 0.046(6) 0.025(5) 0.026(5) 0.007(4) -0.007(4) 0.006(4) N4 0.090(12) 0.086(11) 0.093(12) 0.014(8) -0.003(10) 0.012(10) C1 0.025(6) 0.015(5) 0.035(6) -0.002(4) 0.002(5) -0.008(4) C2 0.020(6) 0.029(6) 0.039(7) -0.003(5) 0.002(5) -0.003(4) C3 0.021(6) 0.027(6) 0.043(7) 0.003(5) 0.001(5) 0.005(5) C4 0.024(6) 0.042(7) 0.027(6) 0.004(5) -0.003(5) -0.001(5) C5 0.024(6) 0.027(6) 0.039(7) 0.001(5) -0.006(5) -0.001(5) C6 0.024(6) 0.025(6) 0.040(7) -0.010(5) -0.004(5) 0.000(5) C7 0.035(6) 0.020(6) 0.038(7) 0.003(5) 0.004(5) 0.005(5) C8 0.057(8) 0.052(8) 0.043(8) 0.015(6) 0.015(7) 0.016(7) C9 0.074(10) 0.043(8) 0.057(9) 0.014(7) 0.016(8) 0.011(7) C10 0.035(6) 0.026(6) 0.030(6) 0.010(5) 0.000(5) -0.002(5) C11 0.056(8) 0.027(6) 0.042(7) 0.005(5) -0.007(6) 0.008(6) C12 0.073(10) 0.032(7) 0.046(8) 0.005(6) 0.010(7) 0.015(6) C13 0.036(6) 0.024(6) 0.033(7) 0.009(5) -0.001(5) -0.004(5) C14 0.054(8) 0.034(7) 0.030(7) -0.002(5) 0.000(6) 0.002(6) C15 0.066(9) 0.053(8) 0.030(7) 0.000(6) -0.002(6) 0.007(7) C16 0.088(13) 0.059(10) 0.058(10) 0.013(8) -0.011(10) 0.023(10) C17 0.088(14) 0.095(14) 0.109(15) -0.028(11) -0.009(12) -0.003(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.929(8) . ? Cu1 N1 1.929(8) 2_655 ? Cu1 Br1 2.412(3) . ? Cu2 N3 1.927(8) . ? Cu2 N2 1.942(8) 5_655 ? Cu2 Br2 2.7326(16) . ? Cu2 Cu3 2.884(2) . ? Br2 Cu3 2.565(4) . ? Br2 Cu2 2.7326(16) 3 ? Cu3 Br4 2.294(2) 3 ? Cu3 Br4 2.294(2) . ? Cu3 Cu2 2.884(2) 3 ? O1 C7 1.336(12) . ? O1 C9 1.462(14) . ? O2 C10 1.353(12) . ? O2 C12 1.457(13) . ? O3 C13 1.341(12) . ? O3 C15 1.455(14) . ? N1 C7 1.283(13) . ? N1 C8 1.474(14) . ? N2 C10 1.255(13) . ? N2 C11 1.488(12) . ? N2 Cu2 1.942(8) 5_655 ? N3 C13 1.279(13) . ? N3 C14 1.474(13) . ? N4 C16 1.09(2) . ? C1 C2 1.374(13) . ? C1 C6 1.375(14) . ? C1 C7 1.474(14) . ? C2 C3 1.393(14) . ? C2 H2A 0.9300 . ? C3 C4 1.399(15) . ? C3 C10 1.466(14) . ? C4 C5 1.400(14) . ? C4 H4A 0.9300 . ? C5 C6 1.410(15) . ? C5 C13 1.435(15) . ? C6 H6A 0.9300 . ? C8 C9 1.518(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.487(16) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.506(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.44(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 143.1(5) . 2_655 ? N1 Cu1 Br1 108.5(3) . . ? N1 Cu1 Br1 108.5(3) 2_655 . ? N3 Cu2 N2 147.8(3) . 5_655 ? N3 Cu2 Br2 106.4(3) . . ? N2 Cu2 Br2 101.4(2) 5_655 . ? N3 Cu2 Cu3 84.2(3) . . ? N2 Cu2 Cu3 126.0(2) 5_655 . ? Br2 Cu2 Cu3 54.26(7) . . ? Cu3 Br2 Cu2 65.88(5) . 3 ? Cu3 Br2 Cu2 65.88(5) . . ? Cu2 Br2 Cu2 131.75(9) 3 . ? Br4 Cu3 Br4 140.26(18) 3 . ? Br4 Cu3 Br2 109.87(9) 3 . ? Br4 Cu3 Br2 109.87(9) . . ? Br4 Cu3 Cu2 133.98(6) 3 . ? Br4 Cu3 Cu2 69.32(5) . . ? Br2 Cu3 Cu2 59.86(6) . . ? Br4 Cu3 Cu2 69.32(5) 3 3 ? Br4 Cu3 Cu2 133.98(6) . 3 ? Br2 Cu3 Cu2 59.86(6) . 3 ? Cu2 Cu3 Cu2 119.72(13) . 3 ? C7 O1 C9 106.8(9) . . ? C10 O2 C12 105.2(8) . . ? C13 O3 C15 107.8(9) . . ? C7 N1 C8 106.9(9) . . ? C7 N1 Cu1 134.4(7) . . ? C8 N1 Cu1 118.6(7) . . ? C10 N2 C11 107.5(8) . . ? C10 N2 Cu2 132.7(7) . 5_655 ? C11 N2 Cu2 117.4(7) . 5_655 ? C13 N3 C14 108.6(9) . . ? C13 N3 Cu2 130.6(8) . . ? C14 N3 Cu2 120.8(7) . . ? C2 C1 C6 120.4(10) . . ? C2 C1 C7 120.7(10) . . ? C6 C1 C7 118.9(9) . . ? C1 C2 C3 121.1(10) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C2 C3 C4 118.9(10) . . ? C2 C3 C10 121.7(10) . . ? C4 C3 C10 119.3(10) . . ? C3 C4 C5 120.4(10) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 118.8(10) . . ? C4 C5 C13 119.3(10) . . ? C6 C5 C13 121.6(9) . . ? C1 C6 C5 120.3(10) . . ? C1 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? N1 C7 O1 117.3(9) . . ? N1 C7 C1 128.4(9) . . ? O1 C7 C1 114.2(9) . . ? N1 C8 C9 104.3(9) . . ? N1 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? N1 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? O1 C9 C8 103.3(9) . . ? O1 C9 H9A 111.1 . . ? C8 C9 H9A 111.1 . . ? O1 C9 H9B 111.1 . . ? C8 C9 H9B 111.1 . . ? H9A C9 H9B 109.1 . . ? N2 C10 O2 117.2(9) . . ? N2 C10 C3 128.4(10) . . ? O2 C10 C3 114.4(9) . . ? C12 C11 N2 103.1(9) . . ? C12 C11 H11A 111.1 . . ? N2 C11 H11A 111.1 . . ? C12 C11 H11B 111.1 . . ? N2 C11 H11B 111.1 . . ? H11A C11 H11B 109.1 . . ? O2 C12 C11 104.7(9) . . ? O2 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? O2 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? N3 C13 O3 115.5(10) . . ? N3 C13 C5 128.8(10) . . ? O3 C13 C5 115.6(9) . . ? N3 C14 C15 103.9(9) . . ? N3 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? N3 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? O3 C15 C14 104.0(9) . . ? O3 C15 H15A 111.0 . . ? C14 C15 H15A 111.0 . . ? O3 C15 H15B 111.0 . . ? C14 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? N4 C16 C17 177(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu2 Br2 Cu3 70.0(3) . . . . ? N2 Cu2 Br2 Cu3 -126.5(3) 5_655 . . . ? N3 Cu2 Br2 Cu2 70.0(3) . . . 3 ? N2 Cu2 Br2 Cu2 -126.5(3) 5_655 . . 3 ? Cu3 Cu2 Br2 Cu2 0.0 . . . 3 ? Cu2 Br2 Cu3 Br4 49.91(5) 3 . . 3 ? Cu2 Br2 Cu3 Br4 -130.09(5) . . . 3 ? Cu2 Br2 Cu3 Br4 -130.09(5) 3 . . . ? Cu2 Br2 Cu3 Br4 49.91(5) . . . . ? Cu2 Br2 Cu3 Cu2 180.0 3 . . . ? Cu2 Br2 Cu3 Cu2 180.0 . . . 3 ? N3 Cu2 Cu3 Br4 -25.9(3) . . . 3 ? N2 Cu2 Cu3 Br4 166.4(3) 5_655 . . 3 ? Br2 Cu2 Cu3 Br4 89.19(17) . . . 3 ? N3 Cu2 Cu3 Br4 115.2(3) . . . . ? N2 Cu2 Cu3 Br4 -52.6(3) 5_655 . . . ? Br2 Cu2 Cu3 Br4 -129.73(7) . . . . ? N3 Cu2 Cu3 Br2 -115.1(3) . . . . ? N2 Cu2 Cu3 Br2 77.2(3) 5_655 . . . ? N3 Cu2 Cu3 Cu2 -115.1(3) . . . 3 ? N2 Cu2 Cu3 Cu2 77.2(3) 5_655 . . 3 ? Br2 Cu2 Cu3 Cu2 0.0 . . . 3 ? N1 Cu1 N1 C7 -24.7(10) 2_655 . . . ? Br1 Cu1 N1 C7 155.3(10) . . . . ? N1 Cu1 N1 C8 157.7(9) 2_655 . . . ? Br1 Cu1 N1 C8 -22.3(9) . . . . ? N2 Cu2 N3 C13 44.5(14) 5_655 . . . ? Br2 Cu2 N3 C13 -166.8(9) . . . . ? Cu3 Cu2 N3 C13 -116.7(10) . . . . ? N2 Cu2 N3 C14 -134.8(8) 5_655 . . . ? Br2 Cu2 N3 C14 13.8(9) . . . . ? Cu3 Cu2 N3 C14 63.9(8) . . . . ? C6 C1 C2 C3 -0.9(15) . . . . ? C7 C1 C2 C3 -179.4(9) . . . . ? C1 C2 C3 C4 0.2(15) . . . . ? C1 C2 C3 C10 176.3(10) . . . . ? C2 C3 C4 C5 0.9(15) . . . . ? C10 C3 C4 C5 -175.3(9) . . . . ? C3 C4 C5 C6 -1.4(15) . . . . ? C3 C4 C5 C13 172.4(10) . . . . ? C2 C1 C6 C5 0.4(15) . . . . ? C7 C1 C6 C5 179.0(9) . . . . ? C4 C5 C6 C1 0.7(15) . . . . ? C13 C5 C6 C1 -172.9(10) . . . . ? C8 N1 C7 O1 -3.4(14) . . . . ? Cu1 N1 C7 O1 178.7(8) . . . . ? C8 N1 C7 C1 179.2(11) . . . . ? Cu1 N1 C7 C1 1.4(19) . . . . ? C9 O1 C7 N1 -4.7(14) . . . . ? C9 O1 C7 C1 173.1(10) . . . . ? C2 C1 C7 N1 -20.8(17) . . . . ? C6 C1 C7 N1 160.7(11) . . . . ? C2 C1 C7 O1 161.8(10) . . . . ? C6 C1 C7 O1 -16.8(14) . . . . ? C7 N1 C8 C9 9.6(13) . . . . ? Cu1 N1 C8 C9 -172.2(8) . . . . ? C7 O1 C9 C8 10.2(14) . . . . ? N1 C8 C9 O1 -11.8(14) . . . . ? C11 N2 C10 O2 -2.9(13) . . . . ? Cu2 N2 C10 O2 158.6(8) 5_655 . . . ? C11 N2 C10 C3 177.9(11) . . . . ? Cu2 N2 C10 C3 -20.6(18) 5_655 . . . ? C12 O2 C10 N2 -7.0(14) . . . . ? C12 O2 C10 C3 172.3(9) . . . . ? C2 C3 C10 N2 -21.8(17) . . . . ? C4 C3 C10 N2 154.4(11) . . . . ? C2 C3 C10 O2 159.0(10) . . . . ? C4 C3 C10 O2 -24.9(14) . . . . ? C10 N2 C11 C12 11.3(13) . . . . ? Cu2 N2 C11 C12 -153.5(8) 5_655 . . . ? C10 O2 C12 C11 13.5(13) . . . . ? N2 C11 C12 O2 -14.8(13) . . . . ? C14 N3 C13 O3 1.7(13) . . . . ? Cu2 N3 C13 O3 -177.7(7) . . . . ? C14 N3 C13 C5 178.5(11) . . . . ? Cu2 N3 C13 C5 -1.0(17) . . . . ? C15 O3 C13 N3 1.8(13) . . . . ? C15 O3 C13 C5 -175.4(10) . . . . ? C4 C5 C13 N3 -148.6(11) . . . . ? C6 C5 C13 N3 25.0(17) . . . . ? C4 C5 C13 O3 28.1(14) . . . . ? C6 C5 C13 O3 -158.3(10) . . . . ? C13 N3 C14 C15 -4.3(12) . . . . ? Cu2 N3 C14 C15 175.3(8) . . . . ? C13 O3 C15 C14 -4.3(13) . . . . ? N3 C14 C15 O3 5.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.870 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.139 #====END